Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 1-(4-chlorophenyl)-1,3-Propanediol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl 3-(4-chlorophenyl)-3-oxopropanoate | HCID 101336 | — |
| 반응물 | Diisopropylaluminium hydride | HCID 21896610 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(4-chlorophenyl)-1,3-Propanediol | HCID 10330082 | 59.5% |
반응 단계
To a solution of 5.0 g of ethyl-4-chlorobenzoylacetate in 100 ml of methylene chloride cooled to -30° C., 77.3 ml of diisopropylaluminium hydride (1.0 mol/l toluene solution) was added, and the resulting mixture was stirred for 30 minutes and then brought back to room temperature over 3 hours, and 4.14 g of methanol and 24.3 g of water were added carefully, and the mixture was stirred for another 1.5 hours. The precipitate was filtered off, and the filtrate was concentrated. The resulting residue was purified by silica gel column chromatography (eluent; n-hexane/ethyl acetate=1/1), to obtain 2.45 g of the title compound as a pale yellow oily substance.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05856327 |
| 출처 데이터셋 | uspto-grants-1999_01 |
| ORD ID | ord-bbbe2d4035484addbe187122e4fa8725 |
| 출처 메모 | uspto-grants-1999_01 |