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Acetonitrile → 1-Benzhydryl-2-(alpha-hydroxybenzyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Hexamethylphosphoramide | HCID 12679 | — |
| 反応物 | Bromodiphenylmethane | HCID 236603 | — |
| 反応物 | Potassium Bicarbonate | HCID 516893 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzhydryl-2-(alpha-hydroxybenzyl)piperidine | HCID 20345280 | — |
反応手順
Reflux under an inert atmosphere for 190 hrs. a stirred suspension of 1.89 g. of erythro-α-(2-piperidyl)phenylmethanol, 2.25 g. of benzhydryl bromide, and 1.00 g. of potassium bicarbonate in 100 ml. of dry acetonitrile containing 14 ml. hexamethylphosphoramide. Cool to room temperature, pour into water, and extract with ether. Wash the extract successively with water and brine and dry over anhydrous sodium sulfate. Acidify the dry ether solution with 4.4 ml. of 1.9 M ethereal HCl. Filter and wash the resultant precipitate with acetone to obtain the analytically pure hydrochloride salt of the title compound, m.p. 232.5°-234° dec.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04173566 |
| 出典データセット | uspto-grants-1979_11 |
| ORD ID | ord-296c1f3357a0401ba648a59243356390 |
| 出典メモ | uspto-grants-1979_11 |