Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide | HCID 59614586 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester | HCID 59614592 | — |
반응 단계
1.4 ml of concentrated sulfuric acid is slowly added to a solution of 4.3 g of N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide in 11 ml of methanol. After stirring 20 hours under reflux, the reaction mixture is allowed to cool down to room temperature and diluted with ice water. Sodium carbonate is added and the aqueous phase is extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated. Chromatography (dichloromethane+1% of ethanol) gave 3.2 g of 1-ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester as a solid, mp: 131-132° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08722578B2 |
| 출처 데이터셋 | uspto-grants-2014_05 |
| ORD ID | ord-5f7ea7b5e80f49749e3f42e2f9de96cb |
| 출처 메모 | uspto-grants-2014_05 |