Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hexane → N,N,5-Trimethyl-4-[(2,3,4,9-tetrahydro-9-methyl-4-oxo-1H-carbazol-3-yl) methyl]-1H-imidazole-1-sulphonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Dimethylsulphamoyl chloride | HCID 83372 | — |
| 반응물 | GR 67330 | HCID 172316 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N,N,5-Trimethyl-4-[(2,3,4,9-tetrahydro-9-methyl-4-oxo-1H-carbazol-3-yl) methyl]-1H-imidazole-1-sulphonamide | HCID 14233929 | — |
반응 단계
A solution of dimethylsulphamoyl chloride (0.16 ml) in dry dichloromethane was added to a stirred solution of 1,2,3,9-tetrahydro-9-methyl-3-[(5-methyl-1H-imidazol-4-yl)methyl]-4H-carbazol-4-one (438 mg) and triethylamine (0.25 ml) in dry dichloromethane (30 ml) and the mixture was heated at reflux for 18 h. After cooling the reaction mixture was adsorbed onto FCC silica which was then applied to a column and FCC eluting with System A (150:8:1) gave an oil, which solidified to a powder on trituration with dry hexane (30 ml). This powder was then further purified by dissolution in dry dichloromethane (30 ml) and crystallisation by addition of dry hexane (10 ml) to give the title compound (518 mg), m.p. 122°-124°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04822881 |
| 출처 데이터셋 | uspto-grants-1989_04 |
| ORD ID | ord-92df16e5fce8404c882045c4791a01ea |
| 출처 메모 | uspto-grants-1989_04 |