Acetic Anhydride → HCID 54045935, Verbindung

HRID 482741Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 482741
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:15][CH:14]([OH:16])[C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[N:11]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:10]1=[O:27])=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:28](OC(=O)C)(=[O:30])[CH3:29]>>[C:28]([O:16][CH:14]1[C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[N:11]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:10](=[O:27])[C@@H:9]([NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH2:15]1)(=[O:30])[CH3:29]

Komponenten

3

Edukt 2

HCID 7918Acetic AnhydrideHCID 13604465HCID 13604465, Verbindung

Produkt 1

HCID 54045935HCID 54045935, Verbindung

Versuchsvorschrift

A solution of 3-(S)-t-butyloxycarbonylamino-1-ethoxycarbonylmethyl-5-hydroxy-2,3,4,5-tetrahydro-1H-[1]benzazepine-2-one (previously described, 1.0 g) in acetic anhydride (20 ml) was maintained at 80° for 3 hours. The reaction mixture was cooled to room temperature and the solvents removed under reduced pressure. Ether (100 ml) was added, and the resulting solution washed with water (50 ml) and dried over magnesium sulfate. The solvent was removed under reduced pressure to give 5-acetoxy-3-(S)-t-butyloxycarbonylamino-1-ethoxycarbonylmethyl-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one as a pale yellow oil which was used without further purification.

Aufarbeitung

  1. customthe solvents removed under reduced pressure
  2. additionEther (100 ml) was added
  3. washthe resulting solution washed with water (50 ml)
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2b8525be92754911870c9eff1e343e2b
Quelldatensatz
uspto-grants-1986_03
Patentnummer
US04575503

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