化工社化工社 化学情報印刷レポート · 研究参考用
Methylenetriphenylphosphorane → 17-Cyclopropylmethyl-3-hydroxy-6-methylene-morphinan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylenetriphenylphosphorane | HCID 137960 | — |
| 反応物 | 17-Cyclopropylmethyl-3-hydroxy-morphinan-6-one | HCID 6602257 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 17-Cyclopropylmethyl-3-hydroxy-6-methylene-morphinan | HCID 54412485 | — |
反応手順
Reaction of 17-cyclopropylmethyl-3-hydroxy-morphinan-6-one (1.58 g, 5 mmole) with methylenetriphenylphosphorane (20 mmole) in dimethyl sulfoxide gave a crude residue which was chromatographed using 10:1 chloroform-methanol containing 1% concentrated ammonium hydroxide. Pure fractions were pooled to give 909 mg (58%) of TR-5609 which crystallized from ethanol to give 532 mg of analytically pure TR-5609, mp 220°-223°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04259329 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-d7ffcb5aa64b450d96fe70fcc9e98e58 |
| 出典メモ | uspto-grants-1981_03 |