Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cyclopropanecarbonyl chloride → 2-Amino-5-bromo-3-cyano-6-fluoro-4-methylphenyl acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile | HCID 86097514 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-Amino-5-bromo-3-cyano-6-fluoro-4-methylphenyl acetate | HCID 86097516 | 97.3% |
반응 단계
2-Amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-75) (7.86 g, 32.08 mmol) and diisopropylethylamine (19.5 ml, 112.2 mmol) were dissolved in ethyl acetate (300 ml), and at 0° C., cyclopropanecarbonyl chloride (4.4 ml, 48.12 mmol) was dropwise added, followed by stirring at room temperature for 16 hours under nitrogen atmosphere. After the reaction, ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine. The organic layer was concentrated under reduced pressure, the resulting residue was recrystallized with diisopropyl ether/ethyl acetate to obtain the entitled compound (8.96 g, 89%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737166B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-26668f8c13a84f17b4fc2b4a1d1a64da |
| 출처 메모 | uspto-grants-2010_06 |