Month: July 2021

Application of 35364-79-5, 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.35364-79-5, name is 2-(3,4-Dichlorophenyl)ethanol, molecular formula is C8H8Cl2O, molecular weight is 191.06, as common compound, the synthetic route is as follows.

General procedure: General procedure: NaBH4 (15 mmol, 3 equiv) was added in portion to a solution of Intermediate 3 (5 mmol) in methanol (200 mL) in an ice bath. The resulting mixture was then warmed to room temperature and stirred for 1 hour. Most of the solvent was evaporated under reduced pressure. Saturated aqueous Na2CCb (50 mL) was added and then the mixture was extracted with EtOAc (3 x 50 mL). Purified from chromatographic column to give alcohol 6 (Scheme 4). The alcohol 6 (0.5 mmol) in DCM (10 mol) was put in ice bath. TEA (0.55 mmol, 1.1 equiv) was added, then methanesulfonyl chloride (0.55 mmol, 1.1 equiv) was added again. The mixture was stirred at 0 C for 2 hours. Removed the DCM and provided crude compound 7 without purification. To a solution of alcohol 4′ (0.5 mmol) and K2CO3 (1 mmol, 2 equiv) in DMF was added mesylate 7 (0.5 mmol). The mixture was stirred overnight at 60 C. Cooled to room temperature and added 50 mL of water. Extracted with EtOAc (2 x 50 mL), Combined the EtOAc layers and washed with brine. Dried (Na2S04), filtered, and concentrated in vacuo. Purified by silica gel chromatography and got the final product II.

Statistics shows that 35364-79-5 is playing an increasingly important role. we look forward to future research findings about 2-(3,4-Dichlorophenyl)ethanol.

Reference:
Patent; UNIVERSITY OF MARYLAND, BALTIMORE; WANG, Hongbing; XUE, Fengtian; LIANG, Dongdong; (178 pag.)WO2018/236856; (2018); A1;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 13726-17-5, name is (4-Chloro-3-methoxyphenyl)methanol, the common compound, a new synthetic route is introduced below. HPLC of Formula: C8H9ClO2

D. Synthesis of 4-chloro-3-methoxybenzaldehyde To a solution of (4-chloro-3-methoxyphenyl)methan-1-ol (5.08 g, 29.4 mmol) in benzene (120 mL) was added MnO2 (5.65 g, 65 mmol). The reaction mixture was refluxed for 17 hr, chilled, and filtered through Celite, washing the cake with CH2Cl2 (300 mL). The filtrate was concentrated in vacuo to give 4-chloro-3-methoxybenzaldehyde (4.5 g, 89%).

The synthetic route of 13726-17-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Portola Pharmaceuticals, Inc.; US6906063; (2005); B2;,
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Synthetic Route of 2807-30-9, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 2807-30-9, name is 2-Propoxyethanol. A new synthetic method of this compound is introduced below.

A 500 ml, round-bottom flask equipped with a 10-tray Oldershaw column and decanting head, thermometer, and a connecting tube with stopcock was charged with 126 grams (1.0 mole) of 3-cyclohexene-1-carboxylic acid, 99 grams (0.95 mole) of 2-propoxyethanol, and 100 ml of toluene. The reaction mass was stirred and brought to reflux. Then 1.1 grams of titanium tetrabutoxide was added via the connecting tube. The temperature of the reaction mass was slowly increased to 200 C. and held at this temperature while removing water and solvent overhead. After a reaction time of 8 hours, the product was cooled and washed with 50 ml of dilute phosphoric acid (10 weight percent in water) and filtered to remove the titanium salts. The organic layer was separated from the water layer, and the organic layer was successively washed with 50 ml portions of a saturated sodium bicarbonate solution and with water. Distillation of the crude product under vacuum through a 12-cm Vigreux column gave 152 grams (75% yield) of 2-propoxyethyl 3-cyclohexenecarboxylate (b.p. 88-90 C. at 2.0 mm Hg) with a chromatographically analyzed purity exceeding 98%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2807-30-9, 2-Propoxyethanol, and friends who are interested can also refer to it.

Reference:
Patent; Union Carbide Chemicals & Plastics Technology Corporation; US5268489; (1993); A;,
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Electric Literature of 575-03-1, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 575-03-1, name is 7-Hydroxy-4-(trifluoromethyl)coumarin. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The appropriate bromoketone (6a-o) (1.7 mmol) and triethylamine (1.6 mmol) were added to as olution of either7-hydroxy-4-methyl-2H-chromen-2-one 4 (1.4 mmol)or 7-hydroxy-4-(trifluoromethyl)-2H-chromen-2-one 5 (1.4 mmol) in THF (20 mL). The mixture was stirred at room temperature for 24h, filtered and the solvent was evaporated under reduced pressure.The solid residue was purified by column chromatography eluting with DCM/MeOH 9:1 to afford (7a-n) and (8a-o).

According to the analysis of related databases, 575-03-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Kandil, Sahar; Westwell, Andrew D.; Mcguigan, Christopher; Bioorganic and Medicinal Chemistry Letters; vol. 26; 8; (2016); p. 2000 – 2004;,
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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. 627-30-5, name is 3-Chloropropan-1-ol, molecular formula is C3H7ClO, 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. Recommanded Product: 627-30-5

Example 1 Preparation of 5-methyl-5-(3-chloropropyl)oxycarboxyl-1,3-dioxan-2-one, (MTCOPrCl), molecular weight 236.65 A catalytic amount (3 drops) of DMF was added to a THF solution (200 mL) of MTCOH (11.1 g, 69 mmol), followed by a solution of oxalyl chloride (7.3 mL, 87 mmol) in THF (100 mL), gently added over 20 min under N2 atmosphere. The solution was stirred for 1 hour, bubbled with N2 flow to remove volatiles, and evaporated under vacuum to give the intermediate MTCCl. A mixture of 3-chloro-1-propanol (5.4 mL, 76 mmol) and pyridine (6.2 mL, 65 mmol) in dry THF (50 mL) was added dropwise to a dry THF solution (100 mL) of the intermediate MTCCl over 30 min, while maintaining a solution temperature below 0 C. with an ice/salt bath. The reaction mixture was kept stirring for another 3 hours at room temperature before it was filtered and the filtrate evaporated. The residue was dissolved in methylene chloride and washed with 1N HCl aqueous solution, saturated NaHCO3 aqueous solution, brine and water, stirred with MgSO4 overnight, and the solvent evaporated. The crude product was passed through a silica gel column by gradient eluting of ethyl acetate and hexane (50/50 to 80/20) to provide the product as a colorless oil that slowly solidified to a white solid (9.8 g, 60%).

With the rapid development of chemical substances, we look forward to future research findings about 627-30-5.

Reference:
Patent; AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH; INTERNATIONAL BUSINESS MACHINES CORPORATION; US2012/231060; (2012); A1;,
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Reference of 1211539-82-0, 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. 1211539-82-0, name is 2,2-Difluorobenzo[d][1,3]dioxol-5-ol, molecular formula is C7H4F2O3, 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 solution of Example 29A (3.0 g, 17.23 mmol) in N,N-dimethylformamide (30 mL) at ambient temperature was added potassium carbonate (4.76 g, 34.5 mmol) and teri-butyl bromoacetate (2.91 mL, 19.82 mmol). This mixture was warmed to 65 C and was allowed to stir for 1.5 hours. The mixture was allowed to cool to ambient temperature and was then partitioned between ethyl acetate (50 mL) and 0 (50 mL). The layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 15 mL). The combined organic fractions were dried over anhydrous Na2SO/t, filtered, and concentrated under reduced pressure to give 5.5 g of teri-butyl 2-((2,2-difluorobenzo[(f][l,3]dioxol-5-yl)oxy)acetate, which was used without further purification. To a mixture of teri-butyl 2-((2,2-difluorobenzo[i ] [l,3]dioxol-5- yl)oxy)acetate (5.0 g, 17.35 mmol) in methanol (60 mL) and water (20.00 mL) was added NaOH (17.35 mL, 87 mmol, 5 M aqueous solution). This mixture was allowed to stir at ambient temperature for 2 hours, and then it was concentrated under reduced pressure. The residue was dissolved in water, and the pH was adjusted to ~1 with 1 N HC1. The resulting solid was collected by filtration to give the title compound (3.28 g, 14.13 mmol, 81% yield) as a white solid. JH NMR (400 MHz, DMSO-<) delta ppm 13.10 (s, 1H), 7.30 (d, / = 8.9 Hz, 1H), 7.13 (d, / = 2.6 Hz, 1H), 6.73 (dd, / = 8.9, 2.6 Hz, 1H), 4.69 (s, 2H). 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 1211539-82-0, 2,2-Difluorobenzo[d][1,3]dioxol-5-ol. Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; MARTIN, Kathleen, Ann; SIDRAUSKI, Carmela; FROST, Jennifer, M.; PLIUSHCHEV, Marina, A.; TONG, Yunsong; BLACK, Lawrence, A.; XU, Xiangdong; SHI, Lei; ZHANG, Qingwei, I.; CHUNG, Seungwon; SWEIS, Ramzi, Farah; DART, Michael, J.; RANDOLPH, John, T.; MURAUSKI, Kathleen; (674 pag.)WO2019/90076; (2019); A1;,
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Reference of 14426-21-2 ,Some common heterocyclic compound, 14426-21-2, molecular formula is C4H12ClNO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

Into a reaction flask equipped with a stirrer, a condenser and a thermometer, 4.84 g (0.01 mol) of intermediate III-2 was added, 30mL dichloromethane to dissolve, add DCC 4. lg, stirring for some time after adding DMAP. After stirring for a period of time, bis (2-hydroxyethyl) amine hydrochloride l.lg (O.Olmol) was added to the reaction system in batches, and the reaction was continued for 2 hours. The filtrate was washed with 3 X 40 mL of water, the dichloromethane layer was separated, dried over anhydrous sodium sulfate, filtered, and evaporated to dryness under reduced pressure. Column chromatography [eluent: nu (petroleum ether) Nu (ethyl acetate) = 90: 10] to give a white solid product of 3.818 (yield 99.8%), yield 66.8%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,14426-21-2, its application will become more common.

Reference:
Patent; Tianjin Pharmaceuticals Research Institute Co., Ltd.; Liu, Ying; Liu, DengKe; Jie, xiaoshuai; Qi, haofei; Wang, jingyang; (13 pag.)CN102838652; (2016); B;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 7541-49-3, name is 3,7,11,15-Tetramethylhexadec-2-en-1-ol. This compound has unique chemical properties. The synthetic route is as follows. COA of Formula: C20H40O

Example 75Synthesis of 1-O-(3,7,11,15-tetramethylhexadec-2-enyl)-D-glucoside 3.4 g (8.7 mmol) of 13-D-Glucose pentaacetate and 2.0 g (6.7 mmol) of phytol were dissolved in dry acetonitrile (7 mL). 1.70 mL (13.4 mmol) of boron trifluoride diethyl etherate complex was added to the solution with cooling on ice. The reaction mixture was allowed to warm up slowly to room temperature while being stirred for 18 hours before addition of 2.8 mL (20 mmol) of triethylamine at 0 C. The resulting solution was diluted with ethyl acetate, and washed with water, 1M hydrochloric acid, saturated sodium bicarbonate aqueous solution, and saturated brine, successively, and dried over sodium sulfate. After filtration, the filtrate was concentrated to obtain a crude product of 1-O-(3,7,11,15-tetramethylhexadec-2-enyl)-D-glucopyranoside tetraacetate.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 7541-49-3, 3,7,11,15-Tetramethylhexadec-2-en-1-ol.

Reference:
Patent; Chemgenesis Incorporated; US2012/264923; (2012); A1;,
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Synthetic Route of 403-41-8, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 403-41-8, name is 1-(4-Fluorophenyl)ethyl Alcohol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A solution of corresponding alcohol 1a,b,d-al (8 mmol), nitroxide 4a (0.085 g, 0.4 mmol) and compound 6d (0.097 g, 0.8 mmol) in CH2Cl2 (10 mL) was added to a vigorously stirred solution of NaHCO3 (2.016 g, 24 mmol) in water (10 mL) at 20 C. Then I2 (4.06 g, 16 mmol) powder was added in one portion to the formed reaction mixture at vigorous stirring and temperature 20-22 C. The reaction mixture was stirred at 20-22 C for appropriate time (see Table 1 in the article). Then, a saturated solution of sodium thiosulfate was added to the stirred reaction mixture for discoloration. Organic and aqueous phases were separated and the aqueous phase was then extracted with CH2Cl2 (3×5 mL). Organic phase and the extracts were combined and washed subsequently with saturated aqueous solution of NaCl (5 mL), aqueous solutionof HCl (1%) saturated with NaCl (3 mL), and then with water (5 mL). The washed extract was dried with anhydrous Na2SO4 and evaporated to dryness to give crude product, which was then purified by vacuum distillation under argon atmosphere or by recrystallization.

According to the analysis of related databases, 403-41-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Kashparova, Vera P.; Klushin, Victor A.; Zhukova, Irina Yu.; Kashparov, Igor S.; Chernysheva, Daria V.; Il’chibaeva, Irina B.; Smirnova, Nina V.; Kagan, Efim Sh.; Chernyshev, Victor M.; Tetrahedron Letters; vol. 58; 36; (2017); p. 3517 – 3521;,
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Related Products of 127-66-2, 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.127-66-2, name is 2-Phenylbut-3-yn-2-ol, molecular formula is C10H10O, molecular weight is 146.19, as common compound, the synthetic route is as follows.

(2-Ethoxybut-3-yn-2-yl)benzene (Table 2, entry 1) [39a]:2-phenyl-3-butyn-2-ol (0.106 g, 0.728 mmol) was added to a 5-mLscrew cap vial and dissolved in CH2Cl2(1 mL). Ethanol (0.036 g,0.897 mmol) was added followed by the addition of [Fc]PF6(0.007 g, 0.022 mmol). The vial was then sealed and heated at40C for 3 days. The solvent was removed and the residue waschromatographed on a neutral alumina oxide (Aluminar®) column(2.5 × 30 cm, hexane and then CH2Cl2) to give the product as a yel-low solid (0.085 g, 0.487 mmol, 67percent). NMR (, CDCl3)1H: 7.67?7.29(m, 7H, aromatic), 3.69 (doublet of quintets, 1 H,2JHH= 7.2 Hz,2JHH= 4.2 Hz, OCHH?), 3.22 (doublet of quintets, 1H,2JHH= 7.2 Hz,2JHH= 4.2 Hz, OCHH?), 2.74 (s, 1H, C CH), 1.78 (s, 3H, CH3), 1.24 (t,3H,2JHH= 7.2 Hz, OCH2CH3) ppm.13C{1H}: 143.3 (s, aromatic ipso),128.6 (s, aromatic), 128.5 (s, aromatic), 127.9 (s, aromatic), 127.6(s, aromatic*), 126.1 (s, aromatic), 84.7 (s, C CH), 75.9 (s, CC CH),75.2 (s, C CH), 60.6 (s, OCH2), 33.2 (s, CH3), 15.6 (s, OCH2CH3)ppm. IR (ATR, Neat): 3284 (m), 3055 (w), 2973 (m), 2926(w), 1714(s), 1670 (s), 1575 (s), 1491 (s), 1335 (s), 1264 (s), 1057 (s), 997 (s)

The chemical industry reduces the impact on the environment during synthesis 127-66-2, I believe this compound will play a more active role in future production and life.

Reference:
Article; Queensen, Matthew J.; Rabus, Jordan M.; Bauer, Eike B.; Journal of Molecular Catalysis A: Chemical; vol. 407; (2015); p. 221 – 229;,
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