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Hydrochloric Acid → 2,3,4,5-Tetrahydro-1H-1-benzazepine-7,9-di-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Water ethanol | HCID 19096565 | — |
| 反応物 | 7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester | HCID 53681205 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,3,4,5-Tetrahydro-1H-1-benzazepine-7,9-di-carboxylic acid | HCID 19797205 | 85% |
反応手順
7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester (3.30 g) and sodium hydroxide (2 g) in a mixed solution of water-ethanol (1:1, 60 ml) was refluxed for 8 hours. After cooled, water (100 ml) was added to the reaction mixture, which was then rendered to have pH 3 with concentrated hydrochloric acid. The deposited crystal was collected by filtration, washed with water and dried to give the intended compound 1.84 g (85.0%), which was then recrystallized from ethanol to give slightly yellow crystal. M.P.: 287°-288° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05242912 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-ca2fd54a918b4c22a80531e0a6588ec9 |
| 出典メモ | uspto-grants-1993_09 |