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[Medz]

Помогите, пожалуйста, найти методики синтеза данного соединения:
4,4-диметокси-3-оксобутиронитрил
(CH3O)2CHCOCH2CN
C(C(CC#N)=O)(OC)OC

C.mol

[mishka]

реаксис
из Methyl dimethoxyacetate + acetonitrile

Stage #1: acetonitrile With sodium methylate In toluene at 90℃; for 1h; Inert atmosphere;
Stage #2: Methyl dimethoxyacetate In toluene at 90℃; for 5h; Solvent; Temperature; Inert atmosphere;

Experimental Procedure
133.01 g
Current Patent Assignee: ZHEJIANG NHU CO., LTD. - CN112939849, 2021, A
Location in patent: Paragraph 0066-0072


Abstract
1-3 Example 1: Preparation of compound I-1
Weigh 82.20g of acetonitrile and 81.03g of sodium methoxide into a 1500mL three-necked flask, and then add 600g of toluene, under the protection of inert gas, raise the temperature to 90°C for stirring reaction. After 1 hour of reaction, add 134.13g of methyl dimethoxyacetate, React at 90°C for 5 hours to stop the reaction. Cool to room temperature, add 200 mL of distilled water and adjust the pH value to 3.0-5.0 with hydrochloric acid, extract three times with ethyl acetate as the extractant, combine the organic phases, perform vacuum distillation (40° C., -0.08 MPa) to recover ethyl acetate. After the recovery is completed, vacuum drying is performed for 4 hours to obtain light yellow liquid compound I-1 133.01g with a purity of 96.85%

в SF таже ссылка

1.1 Reagents: Sodium methoxide
Solvents: Acetonitrile , Toluene ; rt → 90 °C; 1 h, 90 °C
1.2 5 h, 90 °C
1.3 Reagents: Hydrochloric acid
Solvents: Water ; pH 3 - 5
Preparation of (4aS,7aS)-octahydro-1H-pyrrolo[3,4-b]pyridine and its intermediates
By: Fang, Xiang; et al
China, CN112939849 A 2021-06-11

Preparation of (4aS,7aS)-octahydro-1H-pyrrolo[3,4-b]pyridine and its intermediates
By: Fang, Xiang; Krishnamurthy, Dhileepkumar; Wang, Jun; Hu, Ruijun; Zhang, Yongchai; Lu, Liuchun; Guo, Wenlong; Zhao, Lilan; Hu, Xinying
The invention discloses a kind of (4aS,7aS)-octahydro-1H-pyrrolo[3,4-b]pyridine and its intermediates and its preparation method and application. The present invention uses new compound I to V (wherein R1 is C1-4 alkyl) as a key intermediate, develops a new synthetic (4aS,7aS)-octahydro-1H-pyrrolo[3,4-b]pyridine route, used line with dialkoxy acetate as starting raw material, successively through a Claisen condensation, substitution reaction, closing intramol. dehydration ring oxidation, catalytic hydrogenation reduction, chiral separation, dissociation, hydrolysis, intramol. dehydration and closing ring by catalytic hydrogenation to obtain the chiral (4aS,7aS)-octahydro-1H-pyrrolo[3,4-b]pyridine. The preparation technol. of this invention is simple, and overall yield of reaction is high, product quality is good, and technique is environmentally friendly, has good prospects for industrial application.

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https://worldwide.espacenet.com/patent/search?q=CN112939849A

[Medz]

Большое спасибо !!!