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Ammonia → trans-3-Amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Ethyl trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate | HCID 14648534 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | trans-3-Amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide | HCID 14648538 | — |
反応手順
In 600 ml of methanol is dissolved 20 g of ethyl trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate, into which ammonia gas is blown to the level of saturation under ice-cooling. The reaction temperature is slowly elevated to room temperature, and the mixture is allowed to stand still for 24 hours. Then, the reaction mixture is concentrated under reduced pressure. By adding isopropyl alcohol to the obtained residue, crystallization is effected. The crystals are collected by filtration to give 18 g of trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 217°-219° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05055464 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-6b48eddc9d5945a9b371cec852e4480b |
| 出典メモ | uspto-grants-1991_10 |