Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Saccharin → N-(phenylsulfonyl)-benzo-1,2,3-thiadiazole-7-carboxylic acid amide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Saccharin | HCID 5143 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 반응물 | 1,2,3-Benzothiadiazole-7-carbonyl chloride | HCID 18377607 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(phenylsulfonyl)-benzo-1,2,3-thiadiazole-7-carboxylic acid amide | HCID 54415936 | — |
반응 단계
After the addition of a spatula tip of 4-dimethylaminopyridine to a suspension of 4 g of the sodium salt of saccharin in 60 ml of methylene chloride, a solution of 3.9 g of benzo-1,2,3-thiadiazole-7-carboxylic acidchloride in 20 ml of methylene chloride is added dropwise at a maximum of 20° C. The mixture is stirred overnight at room temperature and thenext day the suspension is poured onto ice-water and extracted with ethyl acetate. The extracts are washed with dilute sodium hydrogen carbonate solution and water, dried and concentrated by evaporation. The residue is recrystallised from tetrahydrofuran/hexane to yield the title compound having a melting point of 173°-175° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05051436 |
| 출처 데이터셋 | uspto-grants-1991_09 |
| ORD ID | ord-57fb4903711c4e029181b8fde5791f12 |
| 출처 메모 | uspto-grants-1991_09 |