関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzhydrylamine | HCID 7036 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | (17beta)-3-Oxoandrost-4-ene-17-carboxylic acid | HCID 99472 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 17beta-(N-Diphenylmethylcarbamoyl)androsta-4-ene-3-one | HCID 22862420 | 74% |
反応手順
0.108 ml of benzhydrylamine was added to a solution of 100 mg of androsta-4-ene-3-one-17β-carboxylic acid, a catalytic amount of 4-dimethylaminopyridine and 0.132 ml of triethylamine in 4 ml of methylene chloride. 0.037 ml of methanesulfonyl chloride was divided into three portions and added to this reaction mixture at intervals of 30 minutes at room temperature, whilst stirring. One hour after finishing the addition of methanesulfonyl chloride, the reaction mixture was diluted with methylene chloride, washed with 1N aqueous hydrochloric acid, with water, with an aqueous solution of sodium hydrogencarbonate and with a saturated aqueous solution of sodium chloride, in that order. It was then dried over anhydrous magnesium sulfate, and concentrated by evaporation under reduced pressure. The resulting residue was crystallized from acetone to give 113.2 mg (yield 74%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05717088 |
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| 出典データセット | uspto-grants-1998_02 |
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| ORD ID | ord-8e0d68eed0a54cfaa89e3006b03be0a7 |
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| 出典メモ | uspto-grants-1998_02 |
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