Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dicyclohexylcarbodiimide → 2,6-dichlorophenyl N-[(4,6-dimethoxypyrimidin-2-yl)carbonyl]sulfamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | 4,6-Dimethoxypyrimidine-2-carboxylic acid | HCID 4422483 | — |
| 반응물 | 2,6-Dichlorophenyl sulfamate | HCID 19018467 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,6-dichlorophenyl N-[(4,6-dimethoxypyrimidin-2-yl)carbonyl]sulfamate | HCID 14580660 | — |
반응 단계
2.4 g of 2,6-dichlorophenyl sulfamate are added in portions at 0° C. to 2° C. to a mixture of 2.3 g of dicyclohexylcarbodiimide, 120 mg of 4-dimethylaminopyridine and 2.2 g of 4,6-dimethoxypyrimidine-2-carboxylic acid in 80 ml of absolute dichloromethane, and stirring is continued for 0.5 hour at 0° C. and 3 hours at room temperature. The mixture is filtered off with suction, the organic phase is washed with 100 ml of 1 N hydrochloric acid and then with water and dried over sodium sulfate. The solvent is distilled off, and the residue is recrystallized from diisopropyl ether. This gives 3.2 g of 2,6-dichlorophenyl N-[(4,6-dimethoxypyrimidin-2-yl)carbonyl]sulfamate of melting point 136°-139° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05053072 |
| 출처 데이터셋 | uspto-grants-1991_10 |
| ORD ID | ord-04a6e1e25a904d408478a7344c9b79f6 |
| 출처 메모 | uspto-grants-1991_10 |