Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → (2,6-Dichloro-4-nitrophenyl)methanol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 반응물 | 2,6-Dichloro-4-nitrobenzoyl chloride | HCID 22571681 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | (2,6-Dichloro-4-nitrophenyl)methanol | HCID 23311409 | 26.7% |
반응 단계
Lithium aluminium hydride (400 mg, 10.4 mmol) was added in portions to a stirred solution of 2,6-dichloro-4-nitrobenzoyl chloride (3.0 g, 11.8 mmol) in diethyl ether (50 cm3) at room temperature. After 1.5 h the mixture was poured onto ice (80 g), acidified with 10% sulphuric acid (80 cm3) and extracted with ethyl acetate (3×60 cm3). The dried organic extracts were evaporated to an oil which was purified by chromatography over silica gel with a methanol-dichloromethane solvent gradient. The fractions containing 2,6-dichloro-4-nitrobenzylalcohol, were combined and evaporated under reduced pressure to a give a cream solid mp 111°-4° C. (0.7 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04602041 |
| 출처 데이터셋 | uspto-grants-1986_07 |
| ORD ID | ord-cbd346c2b76c4bf9b973f708636aaa14 |
| 출처 메모 | uspto-grants-1986_07 |