化工社化工社 化学情報印刷レポート · 研究参考用
Dimethoxymethane → 17beta-Acetoxy-3beta-methoxymethoxy-1alpha-methyl-17alpha-n-propyl-5alpha-androstane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethoxymethane | HCID 8020 | — |
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | 17beta-Acetoxy-1alpha-methyl-17alpha-n-propyl-5alpha-androstan-3beta-ol | HCID 70360261 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 17beta-Acetoxy-3beta-methoxymethoxy-1alpha-methyl-17alpha-n-propyl-5alpha-androstane | HCID 70360248 | — |
反応手順
400 mg of 17β-acetoxy-1α-methyl-17α-n-propyl-5α-androstan-3β-ol is combined in 2.8 ml of absolute dichloromethane and 1.8 ml of formaldehyde dimethylacetal with a mixture of 600 mg of kieselguhr W 20 and 300 mg of phosphorus pentoxide and stirred for 45 minutes at room temperature. The mixture is vacuum-filtered from the insoluble components and washed with dichloromethane containing 3-5% triethylamine. The crude product obtained after evaporation is chromatographed on silica gel, thus producing 280 mg of 17β-acetoxy-3β-methoxymethoxy-1α-methyl-17α-n-propyl-5α-androstane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04892867 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-c964f846aaf14c5789db35504ede80cd |
| 出典メモ | uspto-grants-1990_01 |