Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
P-Toluenesulfonamide → 1,3-Dimethyl-5-tosyl-5,6-dihydro-4H-thieno[3,4-c]pyrrole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | P-Toluenesulfonamide | HCID 6269 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3,4-Bis(chloromethyl)-2,5-dimethylthiophene | HCID 288399 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1,3-Dimethyl-5-tosyl-5,6-dihydro-4H-thieno[3,4-c]pyrrole | HCID 18947057 | 63.6% |
반응 단계
A solution of 10 g (0.048 mol) of 3,4-bis(chloromethyl)-2,5-dimethylthiophene and 8.22 g of p-toluenesulphonamide in 600 ml of dry dimethylformamide is added dropwise, over 6 h, to a stirred suspension, heated to 100°-110° C., of 180 g of potassium carbonate in 900 ml of dimethylformamide. After the end of the addition, the mixture is maintained at the same temperature for 30 min, and then filtered. The solid is washed with dimethylformamide. The filtrate is concentrated under vacuum, and the residue is treated with 100 ml of ethanol, and filtered. The solid residue remaining is washed with ethanol and dried. 9.39 g of product are obtained. Melting point: 163°-164° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05380742 |
| 출처 데이터셋 | uspto-grants-1995_01 |
| ORD ID | ord-32ddc447f8a04f45a562d00df4e39c31 |
| 출처 메모 | uspto-grants-1995_01 |