Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzoin → 2,3,5,6,7,8-Hexahydro-2,3-diphenylthiazolo[3,2-a][1,3]-diazepin-3-ol methanesulfonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzoin | HCID 8400 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 1,3-Diazepane-2-thione | HCID 736589 | — |
| 용매 | Acetone | HCID 180 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 2,3,5,6,7,8-Hexahydro-2,3-diphenylthiazolo[3,2-a][1,3]-diazepin-3-ol methanesulfonate | HCID 20528327 | — |
반응 단계
A mixture of 7.75 ml. of methanesulfonyl chloride in 200 ml. of toluene is added, over a period of one hour, to a stirred mixture of 21.2 g. of benzoin, 28 ml. of triethylamine and 100 ml. of toluene. The mixture is allowed to stand 2 hours, 100 ml. of water is added and the emulsion is filtered giving a solid which is washed with water and dried, giving 14.5 g. of benzoin methanesulfonate esters. A 2.90 g. portion of benzoin methanesulfonate esters and 1.30 g. of hexahydro-2H-1,3-diazepin-2-thione are suspended in 50 ml. of warm acetone and heated at reflux for 4 hours. The mixture is cooled, the solid is collected, washed with acetone then ether and dried in vacuo at 60° C., giving 3.9 g. of the desired product, m.p. 176°-178° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04344954 |
| 출처 데이터셋 | uspto-grants-1982_08 |
| ORD ID | ord-064dd7e498d847d686b26da8e63546ce |
| 출처 메모 | uspto-grants-1982_08 |