化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Fluoride → 3beta-Acetoxy-5alpha,6beta-dichloro-14alpha-fluoropregnan-20-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Fluoride | HCID 5235 | — |
| 反応物 | Fluorine | HCID 24524 | — |
| 反応物 | Sodium Trifluoroacetate | HCID 517019 | — |
| 反応物 | 3beta-Acetoxy-5alpha,6beta-dichloropregnan-20-one | HCID 70569121 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Trichlorofluoromethane | HCID 6389 | — |
| 生成物 | 3beta-Acetoxy-5alpha,6beta-dichloro-14alpha-fluoropregnan-20-one | HCID 70569449 | — |
反応手順
3β-Acetoxy-5α,6β-dichloropregnan-20-one (1.4 g) was dissolved in fluorotrichloromethane (250 ml) and chloroform (200 ml) containing sodium trifluoroacetate (ca. 2 g) and sodium fluoride (ca. 2 g). The resulting solution was cooled to -78° and vigourously stirred, whereupon fluorine from four 750 cc bottles (10% v/v fluorine in nitrogen) was bubbled through the solution over a period of 8 hours. The reaction solution was then poured into aqueous sodium thiosulphate and the organic layer was separated, washed with water, dried over potassium carbonate and evaporated to dryness to yield crude 3β-acetoxy-5α,6β-dichloro-14α-fluoropregnan-20-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04284558 |
| 出典データセット | uspto-grants-1981_08 |
| ORD ID | ord-234168b7e3f6491997a2f83d137b1c78 |
| 出典メモ | uspto-grants-1981_08 |