Author: tianli

Application of 2854-16-2, 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 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows.

The compound 4-geo (101.3 mg), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (71.0 mg), and HO-Bt (61.9 mg) were added to methylene chloride (2.1 mL), and the mixed solution was stirred at room temperature under an argon atmosphere for 5 minutes. To the mixed solution was added a methylene chloride solution (1.0 mL) of hydroxyisobutylamine (59.8 g), and the resulting mixed solution was stirred for 4.5 hours. To the mixed solution was added a saturated sodium carbonate aqueous solution, and the water phase was extracted with ethyl acetate. The organic phase was washed with a saturated saline solution. After removing the organic solvent under vacuum, the resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/1?1/2) to obtain 118.0 mg (a yield of 97.5percent) of a yellow viscous oily desired product. Data of the obtained compound are as follows: 1H-NMR (CDCl3, 400 MHz) delta: 1.19-1.34 (1H, m), 1.24 (6H, m), 1.76 (1H, t, J=9.0 Hz), 2.13 (2H, dd, J=6.8, 13.8 Hz), 2.25 (2H, dd, J=6.8, 13.8 Hz), 3.33 (2H, d, J=6.1 Hz), 4.99 (1H, dd, J=4.9, 8.8 Hz), 5.11 (1H, dd, J=4.9, 8.8 Hz), 5.44 (1H, dd, J=9.8, 15.3 Hz), 5.64 (1H, td, J=6.8, 14.9 Hz), 5.81 (1H, d, J=15.3 Hz), 5.83 (1H, s), 6.82 (1H, td, J=6.8, 15.3 Hz); 13C-NMR (CDCl3, 100 MHz), delta: 19.21, 27.35, 31.16, 31.62, 50.45, 56.98, 61.52, 71.10, 81.09, 84.94, 123.77, 130.28, 132.55, 144.20, 166.89; ESI-MS m/z: +ESI 426 [M+Na]+, 404 [M+H]+, -ESI 402 [M-H]-. HRESI-MS m/z: 426.0972 (Calcd for C19H25NO5FeNa: 426.0980). IR (film): cm-1: 3302, 2918, 2035, 1961, 1669, 1627, 622, 610, 571.

According to the analysis of related databases, 2854-16-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TSUMURA & CO.; Aoki, Katsuyuki; US2013/245303; (2013); A1;,
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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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol. A new synthetic method of this compound is introduced below., COA of Formula: C6H15NO

A solution of 1-propanephosphonic acid cyclic anhydride (0.35 rnL) (1.57 M in THF) was added to a suspension of the product of step (i) (69 mg), triethylamine (0.077 mL), 4- (dimethylamino)-l-butanol (0.12 mL) and 4-dimethylaminopyridine (4.50 mg) in DMF (2 mL). The mixture was stirred at r.t. for 60 h and was then diluted with EtOAc (10 mL). The solution was washed with water (2 x 10 mL) dried and concentrated by evaporation. The crude product was purified by RPHPLC to produce a colourless gum which was dissolved in MeCN (0.5 mL). Benzenesulphonic acid (7.9 mg) was added and the solvent was evaporated to give a residue which was triturated with diethyl ether to give the title compound as a colourless solid (27.0 mg); 1H NMR: 7.61-7.58 (m, IH), 7.48-7.45 (m, 3H), 7.34-7.27 (m, 5H), 6.93 (d, IH), 6.21-6.06 (m, IH), 4.63-4.57 (m, IH), 4.27 (t, 2H), 4.20- 4.12 (m, IH), 3.92 (s, 3H), 3.73 (s, 2H), 3.41-3.33 (m, 4H), 2.42 (s, 6H), 2.03 (s, 3H), 1.77- 1.67 (m, 2H), 1.66-1.57 (m, IH), 1.53-1.43 (m, IH), 1.34-1.21 (m, 2H), 1.15-1.03 (m, 2H), 0.77 (t, 3H); LC-MS m/z 474.

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, 13330-96-6, 4-(Dimethylamino)butan-1-ol.

Reference:
Patent; ASTRAZENECA AB; DAINIPPON SUMITOMO PHARMA CO., LTD; ASTRAZENECA UK LIMITED; BENNETT, Nicholas, James; MCINALLY, Thomas; THOM, Stephen; WO2010/133885; (2010); A1;,
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Synthetic Route of 23783-42-8, 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. 23783-42-8, name is 2,5,8,11-Tetraoxatridecan-13-ol. A new synthetic method of this compound is introduced below.

Synthesis of 2,5,8,11-tetraoxatridecan-13-ol tosylate Procedure: [0187] (JACS, 2007, 129, 13364) To a solution of 2,5,8,11-tetraoxatridecan-13-ol (7 g, 33.6 mmol) and triethylamine (4.9 ml, 35.3 mmol) in dry CH2Cl2 (100 ml), 4-toluenesulfonyl chloride (6.7 g, 35.3 mmol) and DMAP (120 mg) were added. The mixture was stirred at room temperature for 20 h. The reaction mixture was washed with 80 mL of HCl (1M) and then water. The extract was dried over anhydrous MgSO4, filtrated, and the filtrate was evaporated. The residue was used in the next step without further purification. Yield: [0188] 11.0 g (90%) NMR: [0189] 1H NMR (400 MHz, CDCl3) delta 7.75-7.64 (m, 2H), 7.31-7.26 (m, 2H), 4.16-4.06 (m, 2H), 3.62 (m 2H), 3.59-3.40 (m, 10H), 3.30 (s, 3H), 2.38 (s, 3H). [0190] 13C{1H} NMR (101 MHz, CDCl3) delta 144.75 (s), 132.90 (s), 129.77 (s), 127.8 (s), 71.82 (s), 70.60 (s), 70.48 (s), 70.47 (s), 70.41 (s), 70.39 (s), 69.23 (s), 68.55 (s), 58.90 (s), 21.53 (s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,23783-42-8, 2,5,8,11-Tetraoxatridecan-13-ol, and friends who are interested can also refer to it.

Reference:
Patent; Bergmann, Frank; Cysewski, Robert; de Cola, Luisa; Dziadek, Sebastian; Fernandez Hernandez, Jesus Miguel; Josel, Hans-Peter; Seidel, Christoph; US2015/147751; (2015); A1;,
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Electric Literature of 96-35-5 ,Some common heterocyclic compound, 96-35-5, molecular formula is C3H6O3, 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.

As a reactive distillation apparatus, an apparatus obtained by connecting a 3-stage packed column to a flask and further providing a refluxing device at the top of the packed column was used. A mixed liquid obtained by mixing 150 g of water with 50 g of the distillate containing more than 98 wt % of methyl glycolate obtained in (3) above was put into the flask. Next, reactive distillation was carried out for 2 hours at normal pressure, maintaining the temperature at the base of the column of the reactive distillation apparatus (i.e. the liquid temperature) at 95 to 97 C. At this time, distillate containing methanol was distilled off. The temperature at the top of the column was 65 C. at the start of the reactive distillation, but had reached 100 C. by the end. [0322] After the reactive distillation had been completed, 114 g of an aqueous solution containing 36.1 wt % of glycolic acid was recovered from the flask. The yield of glycolic acid relative to the methyl glycolate was 100%. Regarding impurities, formaldehyde and chlorine compounds were not detected, and 20 ppm of oxalic acid and 76 ppm of ethylene glycol were detected.

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. 96-35-5, Methyl 2-hydroxyacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hayashi, Toshio; Baba, Hideyuki; US2004/138409; (2004); A1;,
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Electric Literature of 3068-00-6, 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 3068-00-6, name is 1,2,4-Butanetriol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of CoCl2 (0.6 mmol) in anhyd MeCN (4 mL), the selecteddialkyl acetal (1 mmol), TMSCl (1.1 mmol), and butane-1,2,4-triol (3 mmol) were added, with stirring, at r.t. At the end ofthe reaction, the mixture was extracted with EtOAc and the combinedextracts were washed with 5% NaHCO3. The organic layerwas dried (anhyd Na2SO4) and filtered, and the solvent was evaporatedunder vacuum. The oils obtained were purified by flash chromatographyto give the desired compounds.

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 3068-00-6, 1,2,4-Butanetriol.

Reference:
Article; Battisti, Umberto Maria; Sorbi, Claudia; Franchini, Silvia; Tait, Annalisa; Brasili, Livio; Synthesis; vol. 46; 7; (2014); p. 943 – 946;,
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Reference of 307353-32-8, 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.307353-32-8, name is Methyl 3-bromo-5-(hydroxymethyl)benzoate, molecular formula is C9H9BrO3, molecular weight is 245.07, as common compound, the synthetic route is as follows.

A mixture of methyl 3-bromo-5-(hydroxymethyl)benzoate (149 mg, 0.61 mmol) and manganese(IV) oxide (529 mg, 6.08 mmol), and CH2Cl2 (3 mL) was stirred at rt overnight. The mixture was filtered through Celite and the filter cake was washed with CH2Cl2. The filtrate was concentrated to afford the title compound.

The chemical industry reduces the impact on the environment during synthesis 307353-32-8, I believe this compound will play a more active role in future production and life.

Reference:
Patent; RENOVIS, INC.; WO2009/110985; (2009); A2;,
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Application of 4415-73-0, 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.4415-73-0, name is 1,1-Cyclobutanedimethanol, molecular formula is C6H12O2, molecular weight is 116.1583, as common compound, the synthetic route is as follows.

Step 2:Oxalyl chloride (61.5 ml_, 708 mmol) is added over 1.5 h to a -80 C (internal temperature; Et20/dry-ice bath is used for cooling) solution of DMSO (50.2 ml_, 708 mmol) in DCM (3.00 L). The reaction mixture is allowed to stir at -80 C for 0.5 h, and then a solution of 4a1 (30.9 g, 266 mmol) in DCM (500 mL) is added over 1 h while maintaining an internal temperature of -80 C. The reaction mixture is stirred for 0.5 h at -80 C, and then TEA (297 mL, 2.13 mol) is added over 1 h while keeping an internal temperature of -80 C. The cooling bath is removed, and the reaction mixture is allowed to warm to 10 C over 4 h. The crude material containing 4a2 is used as such in the next step.

Statistics shows that 4415-73-0 is playing an increasingly important role. we look forward to future research findings about 1,1-Cyclobutanedimethanol.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BROCHU, Christian; GRAND-MAITRE, Chantal; FADER, Lee; KUHN, Cyrille; BERTRAND-LAPERLE, Megan; PESANT, Marc; WO2013/26163; (2013); A1;,
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Synthetic Route of 6966-10-5, 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. 6966-10-5, name is (3,4-Dimethylphenyl)methanol, molecular formula is C9H12O, 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.

General procedure: A mixture of p-methylbenzyl alcohol (1.0 mmol), N-phenylglycine(0.0076 g, 0.05 mmol), CuBr2 (0.0112 g, 0.05 mmol),Na2CO3 (0.1060 g, 1.0 mmol), TEMPO (0.0078 g, 0.05 mmol),H2O (3.0 mL) were added to a 100 mL Schlenk tube, which wasvigorously stirred in air under reflux for 0.5 h. After the reaction,the product was extracted with CH2Cl2 (3 × 2.0 mL). Thecombined organic phase was washed with H2O (3.0 mL) anddried over anhydrous MgSO4. After concentration undervacuum, the residue was purified by column chromatography toafford p-methylbenzaldehyde.Isolated yield: 0.1080 g (90%).

According to the analysis of related databases, 6966-10-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Guofu; Lei, Jie; Han, Xingwang; Luan, Yuxin; Ding, Chengrong; Shan, Shang; Synlett; vol. 26; 6; (2015); p. 779 – 784;,
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Application of 671802-00-9 ,Some common heterocyclic compound, 671802-00-9, molecular formula is C9H18O4, 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.

Compound 16-3 (2.0 g, 10.5 mmol), N-hydroxyphthalimide (2.05 g, 12.6 mmol) and triphenylphosphine (3.58 g, 13.65 mmol) were dissolved in 50 mL of tetrahydrofuran followed by addition of DIAD (3.26 mL, 15.75 mmol) at 0C. The resulting solution was stirred at room temperature overnight, and then concentrated to dryness. The residue was purified by flash column chromatography to give compound 16-5.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,671802-00-9, its application will become more common.

Reference:
Patent; AMBRX, INC.; MIAO, Zhenwei; ATKINSON, Kyle, C.; BIROC, Sandra; BUSS, Timothy; COOK, Melissa; KRAYNOV, Vadim; MARSDEN, Robin; PINKSTAFF, Jason; SKIDMORE, Lillian; SUN, Ying; SZYDLIK, Angieszka; VALENTA, Ianina; WO2012/166560; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 24034-73-9, (2E,6E,10E)-3,7,11,15-Tetramethylhexadeca-2,6,10,14-tetraen-1-ol, 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, HPLC of Formula: C20H34O, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C20H34O

N–chlorosuccinimide(1.2g,1.3equiv)wassuspendedindryCH2Cl2(15ml).Thesuspensionwascooledto–30C(acetone/liquidN2bath)andafterstirringfor5min,dimethylsulfide(750mul,1.5equiv)wasadded.Thereactionwasstirredfor10minat–30Cand10minat0C.Thenthesolutionwascooledto–40C.Asolutionofgeranylgeraniol(2g,6.9mmol)inCH2Cl2(dry,5ml)wasaddeddropwise.Theresultingsuspensionwasallowedtowarmduring150minto0C,turningintoacloudysolutionat–15C.Thereactionmixturewaspouredintopentane(150ml),Theorganiclayerwaswashedwithwater(2x50ml),brine(50ml),driedoverMgSO4andevaporated.Thereactionafforded1.94gofgeranylgeranylchlorideasacolorlessliquidwhichwasusedwithoutfurtherpurification.

The synthetic route of 24034-73-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jain, Samta; Caforio, Antonella; Fodran, Peter; Lolkema, Juke S.; Minnaard, Adriaan J.; Driessen, Arnold J.M.; Chemistry and Biology; vol. 21; 10; (2014); p. 1392 – 1401;,
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