Author: tianli

Related Products of 13330-96-6, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 13330-96-6 as follows.

General procedure: To a solution of 6-substituted pyridazinone 9 (0.5 mmol) in DMF (10 mL) was added Cs2CO3 (0.55 mmol). An appropriately substituted nitro benzyl chloride (0.52 mmol) was added and the resulting mixture was stirred at 40-50 C for 3 h, the solvent was removed under reduced pressure and the residue was dissolved in EtOAc (30 mL), which was then washed with brine (3 × 10 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product, 2-nitrobenzyl-6-substituted-pyridazin-3(2H)-one (10), was used in the next step without further purification. To a solution of 10 in 95 % ethanol (50 mL) was added acetic acid (10 mmol) followed by slow addition of iron powder (2 mmol). The resulting mixture was stirred for 5 h at 100 C. The mixture was then filtered through celite and the filter cake was washed with 95 % ethanol (3 × 15 mL). The combined ethanol filtrates were evaporated in vacuo and the residue was re-dissolved in ethyl acetate (30 mL). The organic layer was washed with brine (3 × 10 mL) and 2 M NaOH (10 mL) sequentially. The organic layer was dried over anhydrous Na2SO4, evaporated in vacuo to afford 2-aminobenzyl-6-substituted-pyridazin-3(2H)-one (11) as a yellow solid, which was used without further purification. To a stirred solution of 11 and triphosgene (1 mmol) in dry dichloromethane (5 mL) was added triethylamine (2 mmol) under nitrogen atmosphere. A solution of the corresponding alcohol (1 mmol) in dichloromethane (5 mL) was added 5-10 min later and the mixture was stirred at room temperature overnight, diluted with dichloromethane (15 mL) and washed with water (3 × 20 mL). The organic phases were separated, combined, dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by using column chromatography to afford the corresponding product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,13330-96-6, its application will become more common.

Reference:
Article; Xing, Weiqiang; Ai, Jing; Jin, Shiyu; Shi, Zhangxing; Peng, Xia; Wang, Lang; Ji, Yinchun; Lu, Dong; Liu, Yang; Geng, Meiyu; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 95; (2015); p. 302 – 312;,
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Synthetic Route of 349-75-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 349-75-7, name is (3-(Trifluoromethyl)phenyl)methanol, molecular formula is C8H7F3O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

4,6-dimethyl-5-nitro-2-hydroxypyridine (350 mg, 2.08 mmol)Dissolved in 15 mL of dry tetrahydrofuran3-trifluoromethylbenzyl alcohol (0.44 g, 2.50 mmol) was added in the presence of nitrogen,Triphenylphosphine(1.09 g, 4.16 mmol), cooled to 0 C, and azodicarbonyl diisopropyl ester (0.84 mg, 4.16 mmol) was slowly added dropwise. After the drop is finished, the roomStir for three hours. Spin-dried tetrahydrofuran, crude using petroleum ether / ethyl acetate = 30: 1 column to obtain compound 6A, whiteColor solid (589 mg, 86% yield).

According to the analysis of related databases, 349-75-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jiangsu Xiansheng Pharmaceutical Co., Ltd.; Chen Huanming; Liang Bo; Zhao Zhongqiang; Cao Wenjie; Li Amin; Chen Dexin; Gao Chunhua; Zhang Peng; Xu Wanmei; Chen Xuelian; Zhang Lili; (29 pag.)CN103508943; (2017); B;,
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Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-1,3-diol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, COA of Formula: C5H12O2, blongs to alcohols-buliding-blocks compound. COA of Formula: C5H12O2

To a solution of 3-methylbutane-1 ,3-diol (2.5 ml_) in dichloromethane (30 ml_) and pyridine (2.1 ml_) is added at 0C p-toluene-sulfonylchloride (4.6 g) in portions. The mixture is stirred for 12 hours at room temperature, diluted with dichloromethane and washed with 1 M aqueous HCI solution and brine. After drying (MgSO4) the solvent is evaporated and the product is pu rified by ch romatog raphy on s il ica gel (cyclohexane/ethyl acetate 90:10?70:30) to give the title compound. Yield : 3.2 g; Mass spectrum (ESI+): m/z = 276 [M+NH4]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ECKHARDT, Matthias; FRATTINI, Sara; HAMPRECHT, Dieter; HIMMELSBACH, Frank; LANGKOPF, Elke; LINGARD, Iain; PETERS, Stefan; WAGNER, Holger; WO2013/144097; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 27489-62-9, trans-4-Aminocyclohexanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Computed Properties of C6H13NO, blongs to alcohols-buliding-blocks compound. Computed Properties of C6H13NO

Preparation of N-Boc-£r°ws-4-aminocyclohexanolcrystallization IValphans-4-aminocyclohexanol hydrochloride (Aldrich, 96.5g, 0.636 mole) was added with mechanical stirring to 636 mL of 1.0N NaOH in a 3L 3N RBF, equipped with a 50OmL addition runnel. After a clear solution was obtained 30OmL of dioxane was added, and then the misture was cooled in an ice bath to about 50C. A solution of di-tert-butyldicarbonate (Aldrich, 138.9g, 0.636 mole) in dioxane (30OmL) was added to the addition runnel and added dropwise to the reaction mixture over 1 hour. The reaction was then allowed to slowly warm to room temperature with stirring in the bath overnight (milky white mixture). The whole was extracted with EtOAc (I x 80OmL, 2 x 50OmL), the organics were combined and washed with water and brine. At this point the product began to precipitate from the organic layer. 400 mL of ethanol was added to aid solubility of the product. The mixture was dried over magnesium sulfate then filtered and evaporated to 50OmL. Then hexanes (600 mL) was added slowly with stirring. The product, N-Boc-^ralphaMs-4-aminocycIohexanoI, was filtered, and washed thoroughly with hexanes to afford the product as white flakes. (98g, 72%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,27489-62-9, trans-4-Aminocyclohexanol, and friends who are interested can also refer to it.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/62334; (2007); A2;,
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Adding a certain compound to certain chemical reactions, such as: 109-83-1, 2-(Methylamino)ethanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, 109-83-1, blongs to alcohols-buliding-blocks compound. Safety of 2-(Methylamino)ethanol

Example 1 N-(2-hydroxy-ethyl)-4-methoxy-2.6,N-trimethyl-benzenesulphonamide (C) [0152] 3,5-dimethylanisol (A) were dissolved in 50.0 L dichloromethane. After cooling to -35 C. a solution of 17.46 kg (149.85 mol) chlorosulphonic acid in 15.0 L dichloromethane was metered in and the mixture was stirred for about another 30 minutes at -35 C.±5 C. After the reaction was complete 40.0 L of water were metered in at -35 C. to 5 C. and then the organic phase was separated off. The organic phase was diluted with 10.0 L dichloromethane, before a solution of 1.23 kg (14.69 mol) of sodium hydrogen carbonate in 29.0 L water was added. After separation of the organic phase and dilution with 10 L of dichloromethane, a solution consisting of 11.58 kg (154.20 mol) of N-methylaminoethanol (B) in 20.0 L dichloromethane was slowly metered in at 10±5 C. After the reaction was complete, a mixture of 42.0 L water and 4.10 kg (42.59 mol) conc. hydrochloric acid was added, starting at 10 C. The organic phase was separated off, diluted with 10.0 L of dichloromethane and the product ( C) was totally freed from the solvent in vacuo. [0154] Yield: 14.34 kg (71% of theory)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,109-83-1, its application will become more common.

Reference:
Patent; Boehringer Ingelheim International GmbH; Pachur, Thorsten; Pfrengle, Waldemar; Birk, Manfred; Schnaubelt, Juergen; Werthmann, Ulrike; US2013/289049; (2013); A1;,
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Synthetic Route of 5333-42-6, Adding some certain compound to certain chemical reactions, such as: 5333-42-6, name is 2-octyldodecan-1-ol,molecular formula is C20H42O, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 5333-42-6.

Into a 250 ml glass reactor fitted with an Argon purge was placed the hexanoic acid (23.2 grams, 0.2 moles), 2-octyl-1-dodecanol (29.9 grams, 0.1 moles) (Aldrich 97%) (the “C20-alcohol”, which is a Guerbet alcohol) and p-toluene sulfonic acid monohydrate (19 grams, 0.1 mole). The mixture above was purged with Argon at room temperature for one hour. The mixture was then heated to 100 C. under Argon purge for 18 hours. The mixture was then cooled to room temperature. The residue was then dissolved into 100 ml with ethyl acetate and placed into a separatory funnel. The ethyl acetate solution was extracted once with 100 ml of distilled water. The ethyl acetate layer was washed with 250 ml 10 wt % NaHCO3 aqueous solution followed by 250 ml saturated NaCl aqueous solution. The ethyl acetate solution was dried over MgSO4 and then filtered. The ethyl acetate was removed on the rotary evaporator from the solution. The residue from the rotary evaporator was placed on a Kugelrohr vacuum distillation apparatus where the ester was distilled. 1H NMR (CDCl13): delta3.96 (d, 2H, O-CH2-), 2.31 (d, 2H, O=C-CH2-), 1.61-1.26 (m, 39H, -CH2-), 0.80 (t, 9H, CH3). IR (cm-1): 2955, 2925, 2854, 1733, 1466, 1378, 1234, 1168, 1102, 722.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 5333-42-6, 2-octyldodecan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ExxonMobil Chemical Patents Inc.; Patil, Abhimanyu O.; Lewis, Kyle G.; Bodige, Satish; Zushma, Stephen; US2019/62663; (2019); A1;,
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Reference of 90369-75-8, Adding some certain compound to certain chemical reactions, such as: 90369-75-8, name is (3-Chloro-2-methylphenyl)methanol,molecular formula is C8H9ClO, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 90369-75-8.

To a solution of phosphorus tribromide (0.422 mL, 4.47 mmol) in Toluene (30 mL) was added (3-chloro-2-methylphenyl)methanol (2 g, 12.77 mmol). The reaction was stirred at RT overnight. The solvent was removed and the residue was partitioned between EtOAc and brine. The organic layer was concentrated and the residue was purified by biotage (5% EA/hexane) to give the product (2.Og, 71%). 1H NMR (400 MHz, CDC13) deltappm 7.36 (m, IH), 7.24 (m, IH), 7.12 (m, IH), 4.56 (s, 2H). 2.48 (s, 3H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 90369-75-8, (3-Chloro-2-methylphenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXOSMITHKLINE LLC; LIN, Hong; LUENGO, Juan, I.; RIVERO, Ralph, A.; SCHULZ, Mark, James; XIE, Ren; ZENG, Jin; WO2010/135504; (2010); A1;,
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With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.30379-58-9, name is Benzyl 2-hydroxyacetate, molecular formula is C9H10O3, molecular weight is 166.17, as common compound, the synthetic route is as follows.SDS of cas: 30379-58-9

(S)-l -benzyl 2-methyl aziridine-l,2-dicarboxylate (5.105 g, 21.70 mmol), and benzyl 2-hydroxyacetate (6.16 ml, 43.4 mmol) were dissolved in DCM (43.4 ml) and cooled to 0C followed by the addition of BF3.0Et2 (0.275 ml, 2.170 mmol). The reaction was stirred for 2 h. TLC showed the aziridine starting material to be consumed. The reaction was stirred for and additional 14 h. Saturated sodium bicarbonate solution was added to the reaction and the biphasic mixture was vigorously stirred for 20 min. The reaction was diluted with DCM and separated from the aquious phase. The organic layer was washed with brine, dried over sodium sulate and concentrated under vacuum. The crude material was purified by flash chromatography using 10-40% EtOAc/Hexanes. The product fractions were collected and the solvent removed under vacuum to give methyl 0-(2-(benzyloxy)-2-oxoethyl)-N-((benzyloxy)carbonyl)-L-serinate, 3.0 (34%). ESI-MS(+) m/z 402.1 (M+l). NMR (400MHz, CHLOROFORM-d) d 7.43 – 7.30 (m, 10H), 5.95 (d, J=8.0 Hz, IH), 5.18 (s, 2H), 5.15 (s, 2H), 4.50 (dt, J=8.4, 3.1 Hz, IH), 4.12 (d, J=2.8 Hz, 2H), 4.10 – 4.04 (m, IH), 3.81 (dd, J=9.4, 3.1 Hz, IH), 3.77 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,30379-58-9, Benzyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; SUN, Li-Qiang; ZHAO, Qian; MULL, Eric; GILLIS, Eric P.; SCOLA, Paul Michael; (290 pag.)WO2016/57624; (2016); A1;,
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Synthetic Route of 30379-58-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 30379-58-9, name is Benzyl 2-hydroxyacetate, molecular formula is C9H10O3, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a mixture of starting compound 68 (16 g, 41,1 mmol) and benzyl 2 -hydroxy-acetate 77a (13,6 g, 82,2 mmol) in 160 ml DCE was added Sc(OTf)3 (1,41 g, 2,88 mmol). The solution was stirred at 90C for 16 h to achieve complete conversion. The reaction mixture was poured into 200 ml sat. NaHC03 and extracted with 3 x 100 ml DCM. The combined organic phases were dried over anhydrous Na2S04, filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (PE:EtOAc 1:1) and then reverse flash chromatography (neutral), yielding 12,0 g (60 %) of the title compound 78a as yellow oil. MS [M+H]+ (m/z) = 496,0

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 30379-58-9, Benzyl 2-hydroxyacetate.

Reference:
Patent; SANOFI; HOFMEISTER, Armin; JAHN-HORMANN, Kerstin; (0 pag.)WO2019/170731; (2019); A1;,
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Adding a certain compound to certain chemical reactions, such as: 84832-00-8, (5-Amino-2-fluorophenyl)methanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, 84832-00-8, blongs to alcohols-buliding-blocks compound. Quality Control of (5-Amino-2-fluorophenyl)methanol

Example 205 : 1 -(2-Fluoro-5 -morpholinobenzyl)-N-( 1 -methyl- 1 H-pyrazol-4-yl)- 1 H- pyrazo lo [3 ,4-d]pyrimidin-6-amineStep (i) To a solution of 5-Amino-2-fluoro benzyl alcohol (500mg, 3.5mmol) in toluene (12mL) was added DIEA (2eq) and 2-bromoethylether (1.5eq) and the reaction heated to 90C for 18h. The solvent was removed in vacuo and the residue partitioned between EtOAc and H20. The organic phase was dried (Na2S04), filtered and concentrated in vacuo. The resultant residue was purified by column chromatography (petroleum ether: EtOAc) to give 2(2-fluoro-5- morpholinophenyl)methanol (550mg, 74%) as a yellow oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,84832-00-8, its application will become more common.

Reference:
Patent; CELLZOME LIMITED; RAMSDEN, Nigel; HARRISON, Richard John; OXENFORD, Sally; BELL, Kathryn; PITON, Nelly; DAGOSTIN, Claudio; BOUSSARD, Cyrille; RATCLIFFE, Andrew; WO2011/48082; (2011); A1;,
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