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

HRID 464829

Reaktionsgleichung

Reaktionsgleichung von HRID 464829
C(OC([NH:8][C@@H:9]1[C:15](=[O:16])[N:14]([CH2:17][C:18]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])[C:13]2[CH:28]=[CH:29][CH:30]=[CH:31][C:12]=2[O:11][CH2:10]1)=O)(C)(C)C.C(OCC)(=O)C.[ClH:38]>>[ClH:38].[NH2:8][C@@H:9]1[C:15](=[O:16])[N:14]([CH2:17][C:18]([O:20][CH2:21][C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)=[O:19])[C:13]2[CH:28]=[CH:29][CH:30]=[CH:31][C:12]=2[O:11][CH2:10]1

Komponenten

3

Edukt 2

HCID 18599734benzyl 3(S)-tert-butoxycarbonylamino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetateHCID 21866389Hydrogen chloride-ethyl acetate

Produkt 1

HCID 18599732benzyl 3(S)-amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-acetate hydrochloride

Versuchsvorschrift

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.

Aufarbeitung

  1. concentrationThe mixture is concentrated under reduced pressure
  2. customthe resulting residue is crystallized from a mixture of ethyl acetate and ether

Quellen und Nachweise

ORD-Eintrag
ord-9fd1513df6ce4905b6dd814593df7142
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548932

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