Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → 3-Bromo-5-methylbenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 3-Bromo-5-methylbenzoic acid | HCID 3433127 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-Bromo-5-methylbenzamide | HCID 57813398 | 94.2% |
반응 단계
CDI (42.2 g, 260.4 mmol) was cautiously added to a solution of 3-bromo-5-methylbenzoic acid (16.0 g, 74.4 mmol) in EA (300 mL), and then the mixture was kept at reflux for 3 h. After cooled to room temperature, NH3 (g) was passed though for 1 h. The mixture was filtered and the organic layer was washed with HCl (10%, 100 mL) and water (100 mL). The organic phase was dried over Na2SO4 and concentrated in vacuum to obtain 15.0 g of 3-bromo-5-methylbenzamide as white crystals (yield: 94%). 1H NMR (400 MHz, CDCl3): δ 7.73-7.72 (m, 1 H), 7.56-7.55 (m, 1H), 7.50-7.49 (m 1 H), 2.39 (s, 3 H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08067408B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-091fa4daea1343e59aa57325d8ff4317 |
| 출처 메모 | uspto-grants-2011_11 |