Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4,6-Dichloro-n-methylpyrimidin-2-amine → 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4,6-Dichloro-n-methylpyrimidin-2-amine | HCID 259880 | — |
| 반응물 | 4-Chloro-benzenesulfonamide potassium salt | HCID 131721322 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide | HCID 19353555 | 85% |
반응 단계
0.39 g (0.0022 mol) of (4,6-dichloro-pyrimidin-2-yl)-methylamine and 1.0 g (0.0044 mol) of 4-chloro-benzene-sulfonamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 150° C. for 8 hours. Then, the solvent was distilled off in a high vacuum, the residue was partitioned in ethyl acetate/water and extracted. The aqueous phase was saturated with sodium chloride, evaporated briefly in a vacuum, made acid with 4N HCl and extracted with dichloromethane. The two extracts were combined and chromatographed over silica gel with cyclohexane/ethyl acetate 1:1 as the eluent. There was obtained 0.62 g (85%) of 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide as white crystals. m.p. 196-198° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06030976 |
| 출처 데이터셋 | uspto-grants-2000_02 |
| ORD ID | ord-94ca1704d3754db286060055fdd4c10c |
| 출처 메모 | uspto-grants-2000_02 |