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Hydrochloric Acid → 17-cyclobutylmethyl-3-methoxy-8beta-methyl-6-methylene-morphinane Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methylenetriphenylphosphorane | HCID 137960 | — |
| 反応物 | 17-Cyclobutylmethyl-3-methoxy-8beta-methyl-morphinan-6-one | HCID 56616253 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 17-cyclobutylmethyl-3-methoxy-8beta-methyl-6-methylene-morphinane Hydrochloride | HCID 70527923 | 37% |
反応手順
To a solution of methylenetriphenylphosphorane (14.4 mmole) in dimethyl sulfoxide (30 ml) prepared in the usual fashion was added a solution of 17-cyclobutylmethyl-3-methoxy-8β-methyl-morphinan-6-one. The reaction was heated at 75° for 2 hours under an atmosphere of nitrogen. Workup followed by chromatography gave the free base of TR-5377 as a foam. This was converted to the HCl salt which was crystallized from toluene to give 860 mg (37%) of TR-5377, mp. 221°-224°.
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-053c919ec2d24faf9efa89f8a53d82a8 |
| 出典メモ | uspto-grants-1981_03 |