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Hydrogen Sulfide → Thionordiazepam
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Sulfide | HCID 402 | — |
| 反応物 | 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin | HCID 14907886 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Thionordiazepam | HCID 826706 | — |
反応手順
To a stirred solution of 245 mg. (0.5 mmole) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepine in 10 ml. of tetrahydrofuran containing 0.5 ml. of triethylimine at room temperature was introduced a stream of hydrogen sulfide gas until tlc indicated that all the starting material was consumed (15 minutes). Tetrahydrofuran was evaporated. The residue was partitioned between methylene chloride and water. The methylene chloride layer was dried and evaporated. Crystallization of the residue from methanol yielded, in two crops, a product having a melting point of 243°-245°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04739049 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-3003a7854e9646f68410136383523365 |
| 出典メモ | uspto-grants-1988_04 |