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Formamide → Estazolam
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 7-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepine | HCID 12390874 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Estazolam | HCID 3261 | — |
反応手順
To a suspension of 2.8 parts of 7-chloro-2-hydrazino 5-phenyl-3H-1,4-benzodiazepine in 40 parts by volume of formamide is added 1 part by volume of concentrated sulfuric acid. The resulting solution is left standing for 6 hours and then warmed on a boiling water bath for 30 minutes. The solution is diluted with water, neutralized with sodium bicarbonate and extracted with chloroform. The chloroform extract is washed with water and dried over anhydrous sodium sulfate, followed by evaporation of the solvent. The residue is recrystallized from ethyl acetate to give 8-chloro-6-phenyl-4H-s-triazolo [4,3-a][1,4] benzodiazepine as colorless flakes. Melting point: 226° C to 227° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04116956 |
| 出典データセット | uspto-grants-1978_09 |
| ORD ID | ord-d3a6908b9fdc482f960c84e892097c9e |
| 出典メモ | uspto-grants-1978_09 |