Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon Disulfide → Methyl 2-butyl-1-[[2'-(2,5-dihydro-5-thioxo-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl]benzimidazol-7-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | HCID 178418641 | HCID 178418641 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 2-butyl-1-[[2'-(2,5-dihydro-5-thioxo-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl]benzimidazol-7-carboxylate | HCID 10649000 | 32% |
반응 단계
To a mixture of methyl 2-butyl-1-[[2'-(acetoxycarbamimidoyl)biphenyl-4yl)methyl]benzimidazole-7-carboxylate (2.0 g) and CS2 (1.5 g) in DMF (12 ml) gas added sodium hydride (60% in oil, 0.56 g) during a period of 10 minutes and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into ice-water and the pH of the solution was adjusted to 3. The mixture was extracted with ethylacetate and the extract was washed with water, dried, and concentrated to dryness. The residue was crystallized from chloroformmethanol to afford pale yellow prisms (0.64 g, 32 %). m.p. 180°-181° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05243054 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-9265263c0e12469ebf21fb271fd6edfd |
| 출처 메모 | uspto-grants-1993_09 |