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Sulfuric Acid → Estazolam
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 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 | — |
| 反応物 | Ethylorthoformate | HCID 53630039 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Estazolam | HCID 3261 | — |
反応手順
To a solution of 2.0 parts of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine and 7.4 parts of ethyl orthoformate in 80 parts by volume of chloroform is added 2 parts of concentrated sulfuric acid with stirring. The mixture is stirred at room temperature for further 30 minutes, and neutralized with a saturated aqueous sodium bicarbonate solution. Chloroform layer is washed with water and dried over sodium sulfate, followed by distillation of the solvent. Recrystallization of the residue from acetone-n-hexane yields 8-chloro-6-phenyl-4H-s-triazolo-[4,3-a][1,4]benzodiazepine as colorless flakes melting at 226°-227° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04102881 |
| 出典データセット | uspto-grants-1978_07 |
| ORD ID | ord-20254a603c274d94a25071f88736f4d1 |
| 出典メモ | uspto-grants-1978_07 |