Triethylamine → tert-butyl N-(2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)carbamate

HRID 482748Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 482748
[NH2:1][CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[NH:4][C:3]1=[O:13].[C:14]([O:18][C:19](ON=C(C1C=CC=CC=1)C#N)=[O:20])([CH3:17])([CH3:16])[CH3:15].C(N(CC)CC)C>O.O1CCOCC1>[C:14]([O:18][C:19]([NH:1][CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[NH:4][C:3]1=[O:13])=[O:20])([CH3:17])([CH3:16])[CH3:15]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 938652-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrileHCID 44344333-Amino-2,3,4,5-tetrahydro-1H-benzazepin-2-one

Produkt 1

HCID 13243501tert-butyl N-(2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)carbamate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 3-amino-2,3,4,5-tetrahydro-1H[1]benzazepin-2-one (4.0 g), 2-t-butyloxycarbonyloxyimino-2-phenylacetonitrile (6.1 g) and triethylamine (5 ml) in water (20 ml) and dioxane (25 ml) was stirred at room temperature for 18 hours. The resulting solid was filtered off and washed with water. Recrystallization from ethyl acetate gave 3-t-butyloxycarbonylamino-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one, m.p. 199°-201°.

Aufarbeitung

  1. filtrationThe resulting solid was filtered off
  2. washwashed with water
  3. customRecrystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-d2b0010bc2bf4f41acf908b3335decb9
Quelldatensatz
uspto-grants-1986_03
Patentnummer
US04575503

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