Month: July 2021

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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Reference of 756520-66-8, 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. 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol, molecular formula is C8H7Cl2FO, 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: To the solution of compound 6 (17 mg, 0.13 mmol), 3-morpholinopropan-1-ol (19 mg, 0.13 mmol) and PPh3 (51 mg, 0.19 mmol) in anhydrous THF (5 mL) was added 33 uL DEAD (0.19 mmol) dropwise. The reaction mixture was stirred at room temperature for 3h. After completion of reaction, the reaction mixture was concentrated and the residue was purified by silica gel column chromatography using DCM: MeOH=60:1 as eluents.

According to the analysis of related databases, 756520-66-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; An, Xiao-De; Liu, Hongyan; Xu, Zhong-Liang; Jin, Yi; Peng, Xia; Yao, Ying-Ming; Geng, Meiyu; Long, Ya-Qiu; Bioorganic and Medicinal Chemistry Letters; vol. 25; 3; (2015); p. 708 – 716;,
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Electric Literature of 770-71-8 , The common heterocyclic compound, 770-71-8, name is Adamantan-1-ylmethanol, molecular formula is C11H18O, 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.

The adamantane 4-methylbenzenesulfonate was synthesized by reacting adamantyl alcohol (20.5 g, 123 mmol) with p-toluenesulfonic chloride (23.6 g, 123 mmol) in 75 mL of regular DCM, in the presence of 25 mL of triethylamine for 48 hours at room temperature. More DCM was added (100 mL) and the organic layer was washed with water (3×100 mL). Drying, (MgSO4), and evaporation of the solvent gave 34.5 g of tea color oil which under trituration with hexane afforded white solid adamantane 4-methylbenzenesulfonate (30.5 g, 76%).

The synthetic route of 770-71-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NITTO DENKO CORPORATION; RACHWAL, MILA; YAMAMOTO, MICHIHARU; (134 pag.)JP2016/509621; (2016); A;,
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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.431-38-9, name is 3-Amino-1,1,1-trifluoropropan-2-ol, molecular formula is C3H6F3NO, molecular weight is 129.0811, as common compound, the synthetic route is as follows.Recommanded Product: 3-Amino-1,1,1-trifluoropropan-2-ol

General procedure: Sodium triacetoxyhydroborate (900 mg, 4.2 mmol) was added to a solution of 1-naphthaldehyde (2.8 mmol) and the amine (2.8 mmol) in 1,2-dichloroethane (80 mL) at r.t. under nitrogen atmosphere. The reaction mixture was stirred for 6 h at r.t. and was quenched with sat. aq. NaHCO3 (20 mL) and extracted with DCM (3 x 50 mL). The combined organic layer was washed with brine (50 mL), dried and evaporated. The compound was purified by preparative HPLC on a XBridge C18 column (10 m 250×19 ID mm) using a gradient of 30-80% Acetonitrile in H2O/ACN/NH3 95/5/0.2 buffer over 20 minutes with a flow of 19 mL/min. The compounds were detected by UV at 220 nm to provide the product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,431-38-9, 3-Amino-1,1,1-trifluoropropan-2-ol, and friends who are interested can also refer to it.

Reference:
Article; Giordanetto, Fabrizio; Wallberg, Andreas; Ghosal, Saswati; Iliefski, Tommy; Cassel, Johan; Yuan, Zhong-Qing; Von Wachenfeldt, Henrik; Andersen, Soren M.; Inghardt, Tord; Tunek, Anders; Nylander, Sven; Bioorganic and medicinal chemistry letters; vol. 22; 21; (2012); p. 6671 – 6676,6;,
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