Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus oxychloride → 3-Ethoxy-4-methoxybenzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 3-Ethoxy-4-methoxybenzamide | HCID 5005106 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 3-Ethoxy-4-methoxybenzonitrile | HCID 3934769 | 94.5% |
반응 단계
To a solution of 3-ethoxy-4-methoxybenzamide (3.30 g) in pyridine (33 mL) was added phosphorus oxychloride (1.73 mL) under ice-water cooling, and the mixture was stirred for 2 hours at ambient temperature. After evaporation of the solvent, the residue was partitioned between ethyl acetate and water under ice-water cooling. The separated organic layer was washed with 1N-hydrochloric acid, water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by a silica gel column chromatography eluting with a mixture of hexane and ethyl acetate (5:1 to 4:1) to give 3-ethoxy-4-methoxybenzonitrile as colorless powders (2.83 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06384080B1 |
| 출처 데이터셋 | uspto-grants-2002_05 |
| ORD ID | ord-63c688fd1ad0413283b1898f3a43d50c |
| 출처 메모 | uspto-grants-2002_05 |