化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3-Hydroxy-2-methoxy-estra-1,3,5(10)-triene-17-thione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | 2-Methoxyestrone | HCID 440624 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-Hydroxy-2-methoxy-estra-1,3,5(10)-triene-17-thione | HCID 11594854 | 36% |
反応手順
A solution of 1.09 g (3.63 mmol) of 3-hydroxy-2-methoxy-estra-1,3,5(10)-trien-17-one in 60 ml of toluene (abs.) was mixed with 3.7 g of Lawesson's reagent, and it was refluxed for four hours. After water was added, it was extracted with dichloromethane (3×), and the combined organic phases were washed with water, dried on sodium sulfate, and concentrated by evaporation in a rotary evaporator. Flash chromatography (n-hexane/ethyl acetate) yielded 412 mg (36%) of the desired product as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07419972B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-2b87ae866ad34a3a88f8e4d53d11a509 |
| 出典メモ | uspto-grants-2008_09 |