참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Chlorobenzoyl chloride | HCID 8501 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | HCID 178418401 | HCID 178418401 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178418352 | HCID 178418352 | — |
반응 단계
A solution of 1.0 g (0.0043 mol) of trans-4-(4-dimethylaminomethylphenyl)-cyclohexanol and 0.6 ml of triethylamine in 50 ml of methylene chloride is combined, dropwise, with 0.75 g (0.0043 mol) of 4-chlorobenzoylchloride, with stirring, and refluxed for 3 hours. After cooling, 50 ml of water are added, the mixture is adjusted to pH 12-13 with sodium hydroxide solution, the methylene chloride phase is separated off and the aqueous phase is extracted once more with methylene chloride. The combined organic phases are dried over sodium sulphate and evaporated down in vacuo. The solid residue is purified by column chromatography (aluminium oxide neutral, activity stage III, ICN; petroleum ether/ethyl acetate=40:1). White crystals are obtained with a melting point of 94°-95° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05726205 |
|---|
| 출처 데이터셋 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-fe8da988a6f64ed0968009c91353edde |
|---|
| 출처 메모 | uspto-grants-1998_03 |
|---|
