Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Hydroxybenzaldehyde → 3-(2,2,2-Trichloro-1-hydroxyethyl)phenol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Hydroxybenzaldehyde | HCID 101 | — |
| 반응물 | Carbon Tetrachloride | HCID 5943 | — |
| 반응물 | Lead (II) bromide | HCID 24831 | — |
| 반응물 | Aluminum | HCID 5359268 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-(2,2,2-Trichloro-1-hydroxyethyl)phenol | HCID 68748571 | 91% |
반응 단계
Aluminum (8.06 g, 0.3 mol) and lead bromide (3.7 g, 0.01 mmol) were added to a mixture of 3-hydroxy benzaldehyde (12.3 g, 0.1 mol) was mixed with 200 ml of dimethylformamide. Carbon tetrachloride (61.53 g, 0.4 mol) was slowly added thereto, the mixture was stirred at room temperature for 10 hours, and unreacted solid was filtered to remove therefrom. After sequentially adding 5% HCl, ethylacetate and water thereto, the mixture was extracted three times with ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate, filtered and distilled. The resulting residue was subjected to column chromatography (ethyl acetate:n-hexane=1:4) to obtain the title compound (12.57 g, 91%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08410302B2 |
| 출처 데이터셋 | uspto-grants-2013_04 |
| ORD ID | ord-8a07bd8b52cc420d9a7b30a37fd6afd6 |
| 출처 메모 | uspto-grants-2013_04 |