Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine, hydrochloride → 3-Cyano-4-dimethylamino-benzoic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methyl 3-cyano-4-fluorobenzoate | HCID 45790123 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 3-Cyano-4-dimethylamino-benzoic acid methyl ester | HCID 59847657 | 94% |
반응 단계
To a stirred solution of 24.0 g (134 mmol) 2 and 240 ml dimethylsulphoxid were added 13.2 g (161 mmol) dimethylamine hydrochloride and 38.9 g (281 mmol) potassium carbonate. The reaction mixture was stirred over night and was reduced with high vacuum rotation evaporator at 65° C. The residue was diluted with dichloromethane, washed twice with water. The combined water phases were extracted with dichloromethane. The combined dichloromethane phases were washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The oily crude product 3 was obtained in 94% yield (25.7 g, 126 mmol) and was used for the next step without purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08557776B2 |
| 출처 데이터셋 | uspto-grants-2013_10 |
| ORD ID | ord-5b67f8c4f0ab4efc806f2630b0eb3865 |
| 출처 메모 | uspto-grants-2013_10 |