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benzyl 3(S)-tert-butoxycarbonylamino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate → benzyl 3(S)-amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | benzyl 3(S)-tert-butoxycarbonylamino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate | HCID 18599734 | — |
| 反応物 | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| 生成物 | benzyl 3(S)-amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate hydrochloride | HCID 18599732 | — |
反応手順
To 7.6 g of benzyl 3(S)-tert-butoxycarbonylamino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate is added 30 ml of hydrogen chloride-ethyl acetate solution (5N) and the mixture stands for 3 hours at room temperature. The mixture is concentrated under reduced pressure and the resulting residue is crystallized from a mixture of ethyl acetate and ether to give 6.2 g of benzyl 3(S)-amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate hydrochloride as a colorless crystalline powder, melting at 169°-172° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04591458 |
| 出典データセット | uspto-grants-1986_05 |
| ORD ID | ord-4c5bc37ced1e4054a48fd12113a7b940 |
| 出典メモ | uspto-grants-1986_05 |