Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 3-(2-Cyano-acetyl)-3-methyl-1-(2-isocyanobenzyl)-urea
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Cyanoacetic acid | HCID 9740 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 1-(2-Isocyanobenzyl)-3-methylurea | HCID 58076127 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Propan-2-ol--water (1/1) | HCID 21889133 | — |
| 생성물 | 3-(2-Cyano-acetyl)-3-methyl-1-(2-isocyanobenzyl)-urea | HCID 58076124 | 68% |
반응 단계
Under nitrogen atmosphere, 1-(2-isocyanobenzyl)-3-methylurea (98.4 g) and cyanoacetic acid (80.0 g) was added to N,N-dimethylformamide (836 ml). The mixture was stirred at room temperature and methanesulfonyl chloride (72.8 ml) was added dropwise with stirring at this temperature. The mixture was stirred at room temperature for 4 hrs, cooled with water, and water-isopropanol [2:1 (volume ratio), 1670 ml] was added drop wise. The mixture was stirred under water-cooling for 1 hr, and the precipitated crystals were collected by filtration and dried to give 3-(2-cyano-acetyl)-3-methyl-1-(2-isocyanobenzyl)-urea with 68% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08841447B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-2d62973b998f4ada92c1a893133f91ed |
| 출처 메모 | uspto-grants-2014_09 |