Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanamine, N-methoxy-, hydrochloride (1:1) → 4-fluoro-3-hydroxy-N-methoxy-N-methylbenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | 4-Fluoro-3-hydroxybenzoic acid | HCID 593635 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-fluoro-3-hydroxy-N-methoxy-N-methylbenzamide | HCID 59459052 | 100% |
반응 단계
To a solution of 4-fluoro-3-hydroxybenzoic acid (1.49 g, 9.55 mmol) in DCM (40 mL) was added TEA (1.2 mL, 8.61 mmol) followed by N,O-dimethylhydroxylamine hydrochloride (1.12 g, 11.5 mmol). The reaction mixture was stirred at room temperature for 3 h, then diluted with DCM, washed with water twice, dried over Na2SO4, filtered and concentrated to yield 4-fluoro-3-hydroxy-N-methoxy-N-methylbenzamide as a colorless oil (1.90 g, 100% yield). LCMS: RT=0.89 min [M+H] 200.10 (Phenomenex Luna C18 column, 4.6×30 mm eluting with 10-90% MeOH/H2O over 2 minutes containing 0.1% TFA; 5 mL/min, monitoring at 220 nm).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08642576B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-a63353c108514aaa90368f012e009f9a |
| 출처 메모 | uspto-grants-2014_02 |