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Isopropanol → Medazepam
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Hexamethylenetetramine | HCID 4101 | — |
| 反応物 | Ammonium Bromide | HCID 25514 | — |
| 反応物 | 2-(2-Ethyl-methylamino)-5-chlorobenzophenone | HCID 57101088 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Medazepam | HCID 4041 | — |
反応手順
Reflux 0.005 moles of 2-(2-ethyl-methylamino)-5-chlorobenzophenone, 0.020 moles of hexamethylenetetramine and 0.020 moles of ammonium bromide together for 2 hours in 14 ml. of 85% (v/v) aqueous isopropyl alcohol. Pour the reaction mixture into water and extract the product with benzene. Wash the benzene solution with water, dry over anhydrous sodium sulfate, filter and evaporate to dryness. After recrystallization, 7-chloro-2,3-dihydro-1-methyl-5-phenyl-1H-1,4-benzodiazepine is obtained. The material gives a single spot by thin layer chromatography, and after drying under vacuum at 110° C., shows no depression on mixed melting point with an authentic sample.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04155904 |
| 出典データセット | uspto-grants-1979_05 |
| ORD ID | ord-5985d48a684e429081cc14650201402b |
| 出典メモ | uspto-grants-1979_05 |