化工社化工社 化学情報印刷レポート · 研究参考用
Water → Atamestane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium Carbonate | HCID 11125 | — |
| 反応物 | 2beta-Iodo-1alpha-methylandrost-4-ene-3,17-dione | HCID 11144378 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Atamestane | HCID 57050 | — |
反応手順
2.13 g (5 mmol) of 2β-iodo-1α-methylandrost-4-ene-3,17-dione of example 1 is introduced in a suspension of 0.73 g (10 mmol) of lithium carbonate in 10 ml of dimethylformamide preheated to 130° C. and stirred for 1.5 hours at this temperature. After cooling, the reaction solution is added to 30 ml of water, extracted with ethyl acetate and after drying on sodium sulfate, concentrated by evaporation. The crude product is chromatographed on silica gel with ethyl acetate/hexane as mobile solvent. After recrystallization from ethyl acetate, 1.1 g of 1-methylandrosta-1,4-diene-3,17-dione (74% of theory) of melting point 169° C. is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05391778 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-aa91c1a6b35442468f6d75d761b5b33b |
| 出典メモ | uspto-grants-1995_02 |