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Water → 2beta-(1,4-Dioxa-8-azaspiro[4.5]dec-8-yl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| 反応物 | 2Alpha,3alpha-epoxy-16beta-(1-pyrrolidinyl)-5alpha-androstan-17beta-OL | HCID 16063872 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2beta-(1,4-Dioxa-8-azaspiro[4.5]dec-8-yl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol | HCID 22868545 | — |
反応手順
After adding 63 g of 1,4-dioxa-8-azaspiro[4.5]decane and 13 ml of water to 17 g of 2α,3α-epoxy-16β-(1-pyrrolidinyl)-5α-androstane-17β-ol, the reaction mixture is maintained at 100° to 105° C. for 80 hours while introducing nitrogen. After completion of the reaction, the solution containing a precipitate is diluted with 200 ml of acetonitrile and after filtering, the precipitate is thoroughly washed with water and then with acetonitrile, dried and recrystallized from methanol to give the title product in a yield of 18.2 g (76.5%), m.p.: 184°-187° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05591735 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-d432d9d21a9f4e12b3cc1722ac9e8480 |
| 出典メモ | uspto-grants-1997_01 |