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Methanol → (S)-1,3,4,5-Tetrahydro-4-amino-3-oxo-2 H-2-benzazepine-2-acetic acid, ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | (S)-1,3,4,5-tetrahydro-4-[[(phenylmethoxy)carbonyl]amino]-3-oxo-2H-2-benzazepine-2-acetic acid, ethyl ester | HCID 86749789 | — |
| 触媒 | Palladium hydroxide | HCID 9942167 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (S)-1,3,4,5-Tetrahydro-4-amino-3-oxo-2 H-2-benzazepine-2-acetic acid, ethyl ester | HCID 86749788 | — |
反応手順
20% Palladium hydroxide/carbon catalyst was added to a solution of (S)-1,3,4,5-tetrahydro-4-[[(phenylmethoxy)carbonyl]amino]-3-oxo-2H-2-benzazepine-2-acetic acid, ethyl ester (1.037 g., 2.62 mmole) in absolute ethanol (20 ml.) and the resulting suspension was stirred under a hydrogen atmosphere (balloon) for 2 hours. The mixture was filtered through Celite and filtrate was evaporated to dryness. The semi-solid residue was triturated with hexane to give 0.63 g. of product as a white, crystalline solid; m.p. 71°-73° C.; Rf =0.38 (methanol:methylene chloride, 1:9); [α]D =77.5° (c=0.59, chloroform).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723602 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-d232c1adede245b1b40453d6829ded7a |
| 出典メモ | uspto-grants-1998_03 |