Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 6-Chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfinyl chloride | HCID 548463 | — |
| 반응물 | HCID 10198105 | HCID 10198105 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6-Chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine | HCID 9881666 | — |
반응 단계
A solution of methanesulphinyl chloride (0.98 g) in dichloromethane (10 ml) was added dropwise at room temperature to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (1.99 g, prepared in a similar manner to its hydrochloride, Example 1 above) and triethylamine (1.01 g) in dichloromethane (50 ml). The reaction mixture was stirred at room temperature for one hour, washed with water, dried and the solvent was removed by evaporation. Purification of the residue by flash chromatography using dichloromethane/ethanol (98:2) as eluent gave 6-chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from ethylacetate/hexane. Yield 2.1 g (m.p. 82°-84° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05580866 |
| 출처 데이터셋 | uspto-grants-1996_12 |
| ORD ID | ord-a4b39ac55d1746fba3b43ffd23dfb566 |
| 출처 메모 | uspto-grants-1996_12 |