Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 5-[4-(6,11-Dihydrodibenzo[b,e]thiepin-11-ylidene)piperidino]-2-pentanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Pentanone, 5-bromo- | HCID 77493 | — |
| 반응물 | 4-dibenzo[b,e]thiepin-11(6H)-ylidenepiperidine | HCID 15077940 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 5-[4-(6,11-Dihydrodibenzo[b,e]thiepin-11-ylidene)piperidino]-2-pentanone | HCID 20371506 | — |
반응 단계
A solution of 10 g of 5-bromo-2-pentanone in 40 cc of chloroform is added dropwise within 10 minutes to a mixture of 14.7 g of 4-(6,11-dihydrodibenzo[b,e]thiepin-11-ylidene)piperidine and 12.7 g of potassium carbonate in 200 cc of chloroform, and the mixture is heated at reflux for 18 hours. After cooling, filtration is effected, the filtrate is washed with water, dried over magnesium sulphate, and the solvent is completely removed by distillation. The oily residue is then chromatographed on 200 g of silica gel with a mixture of chloroform/ethanol 9:1, and the so purified title compound is converted into the hydrogen fumarate form. M.P. 215°-218° from ethanol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04072756 |
| 출처 데이터셋 | uspto-grants-1978_02 |
| ORD ID | ord-49a090cdd1654cd6bdbb4e1731208c2c |
| 출처 메모 | uspto-grants-1978_02 |