Introduction of a new synthetic route about 10203-58-4

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, Diethyl isobutylmalonate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 10203-58-4, The chemical industry reduces the impact on the environment during synthesis 10203-58-4, name is Diethyl isobutylmalonate, I believe this compound will play a more active role in future production and life.

To a solution of 8.34 g (38.6 mmol) of diethyl isobutylmalonate in 35 mL of 95% EtOH was added a solution of 9.0 g (161 mmol) of KOH in 110 mL of 95% EtOH. The mixture was stirred at 25 C. for 16 hours and then at reflux for 1 hour. The mixture was cooled, diluted with water and extracted with CH3 Cl. The aqueous layer was cooled to 0 C. and acidified to pH<1 with 30 mL of concentrated HCl, then it was extracted with CHCl3. The aqueous layer was further continuously extracted with CHCl3 overnight. The combined organic extracts were dried over anhydrous Na2 SO4 and evaporated to afford 5.44 g (33.9 mmol, 88%) of isobutylmalonic acid as a solid which was essentially pure according to 1 H NMR and which was used without further purification. Characteristic analytical data are as follows: mp 108-110 C.; 1 H NMR (300 MHz, CDCl3) delta3.52 (t, J=8 Hz, 1H), 1.84 (t, J=8 Hz, 2H), 1.66 (m, 1H), 0.94 (d, J-7 Hz, 6H); 13 C NMR (75 MHz, CDCl3) delta175.6 (C=O), 49.7 (CH), 37.1 (CH2), 25.7 (CH), 21.7 (CH3). 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, Diethyl isobutylmalonate, other downstream synthetic routes, hurry up and to see. Reference:
Patent; Florida State University; US5470834; (1995); A;,
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New learning discoveries about 10203-58-4

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

Reference of 10203-58-4,Some common heterocyclic compound, 10203-58-4, name is Diethyl isobutylmalonate, molecular formula is C11H20O4, 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.

(b) 2-(S-Acetylthiomethyl)4-methylpentanoic acid Hydrolysis of 91.1 g of isobutyldiethyl malonate is accomplished by digesting a solution of the ester in 300 ml of methanol and 400 ml of 10% NaOH for 6 hours at 80 C. The solution is concentrated in vacuo to 400 ml. It is acidified with 10% aqueous HCl and product is extracted with ethyl acetate to yield 67.6 g of the diacid. This crystallized on standing. M.P. 94-95 C. The diacid is suspended in 400 ml of water and cooled to 5 C. Aqueous 40% dimethylamine (50 g) and aqueous 37% formaldehyde (35.7 g) are added in that order. The solution is stirred overnight and Mannich base solid product is filtered and dried in vacuo to yield 57.3 g. M.P. 134-137 C. with CO2 and dimethylamine given off. The Mannich base (57.3 g) is suspended in 200 ml of water and 43 g of 50% NaOH in 100 ml of water is added until pH is 9. This solution is heated on the steam cone under nitrogen overnight. It is neutralized with 10% HCl and product is extracted with ethyl acetate to yield 23.8 g. The crude unsaturated acid is chromatographed (twice) on 200 g of silica to give 21.6 g of pure acid.

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

Reference:
Patent; E. R. Squibb & Sons, Inc.; US4382081; (1983); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Introduction of a new synthetic route about Diethyl isobutylmalonate

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10203-58-4, 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. 10203-58-4, name is Diethyl isobutylmalonate, This compound has unique chemical properties. The synthetic route is as follows.

2-aminotetrahydropyrrolidine hydrochloride (1.33 g, 10 mmoL) was dissolved in 60 mL of anhydrous ethanol, and 1.33 mL of triethylamine was added dropwise with constant stirring, and the reaction was carried out for 10 min at room temperature.A solution of sodium ethoxide (1.36 g, 20 mmoL) in absolute ethanol (20 mL) was added dropwise on an ice bath and allowed to react for 45 min at room temperature after the addition was complete.A solution of diethyl isobutyl malonate (2.16 g, 10 mmoL) in absolute ethanol (20 mL) was added dropwise with constant stirring, and the temperature was raised and refluxed for 15 hours.After TLC tracking, after the reaction was completed, the mixture was filtered by suction and the filtrate was collected. The filtrate was evaporated and the solvent was removed to give a yellow solid.100 mL of water was dissolved and 100 mL of ethyl acetate was extracted three times. Fat-soluble impurities were removed and the aqueous phases were combined.Butanol was extracted and the n-butanol layer was collected, rotary evaporated and the solvent removed to give a pale yellow solid.The trichloromethane was dissolved, suction filtered to remove impurities that were insoluble in chloroform, and the filtrate was collected and spin-dryed to give a white solid as the compound 3-isobutyl-tetrahydropyrrole [1,2-a]pyrimidine-2, 4(1H,3H)-dione.

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Reference:
Patent; Xi’an Jiaotong University; Guo Zengjun; Li Dandan; Zhang Jie; Zhang Hui; Liu Xia; Li Mengyi; Xi Ke; (13 pag.)CN104693205; (2017); B;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics