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Sulfuric Acid → Alprazolam
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 | Ethyl ortho-acetate | HCID 86598186 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Alprazolam | HCID 2118 | — |
反応手順
To a suspension of 2.84 parts of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine in a mixture of 100 parts by volume of ethanol and 5 parts by volume of ethyl orthoacetate is added 1 part of concentrated sulfuric acid with stirring. The mixture is further stirred for 30 minutes, and about 100 parts by volume of a saturated aqueous sodium bicarbonate solution is added. The mixture is concentrated under reduced pressure. The resulting crystals are collected by filtration, washed with water and dried to give 8-chloro-1-methyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine as colorless crystals. Recrystallization from acetone-n-hexane gives colorless needles 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-7191ab0e30e746728ee43581e9355792 |
| 出典メモ | uspto-grants-1978_07 |