化工社化工社 化学情報印刷レポート · 研究参考用
Triphenylphosphine → 3alpha-Azido-5alpha-pregnan-20-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Isopregnanolone | HCID 92787 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3alpha-Azido-5alpha-pregnan-20-one | HCID 9946060 | — |
反応手順
A solution of 3β-hydroxy-5α-pregnan-20-one (60 mg, 0.19 mmol) in THF (2 mL) was treated with triphenylphosphine (100 mg, 0.38 mmol) and diethyl azo-dicarboxylate (0.03 mL, 0.19 mmol). To the resulting solution was added dropwise diphenylphosphoryl azide (0.04 mL, 0.19 mmol) and the mixture was stirred at RT for 24 h. Evaporation of the solvent in vacuo and purification of the residue using flash column chromatography using petroleum ether/ethyl acetate 90/10 as elution solvent afforded the compound named above.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07064116B2 |
| 出典データセット | uspto-grants-2006_06 |
| ORD ID | ord-50ff6a499e1248a5b68789a496cc640e |
| 出典メモ | uspto-grants-2006_06 |