Diethyl Ether → N-[2-(1H-Imidazol-2-yl)ethyl]-2-[[3-(1,1-dimethylethyl)-benzoyl]amino]benzamide

HRID 1608837Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1608837
[NH2:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][C:9]1[NH:10][CH:11]=[CH:12][N:13]=1)=[O:5].[C:18]([C:22]1[CH:23]=[C:24]([CH:28]=[CH:29][CH:30]=1)[C:25](Cl)=[O:26])([CH3:21])([CH3:20])[CH3:19].C(OCC)C>CO.C(OCC)(=O)C>[NH:13]1[CH:12]=[CH:11][N:10]=[C:9]1[CH2:8][CH2:7][NH:6][C:4](=[O:5])[C:3]1[CH:14]=[CH:15][CH:16]=[CH:17][C:2]=1[NH:1][C:25](=[O:26])[C:24]1[CH:28]=[CH:29][CH:30]=[C:22]([C:18]([CH3:20])([CH3:19])[CH3:21])[CH:23]=1

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 200855782-Amino-N-[2-(1H-imidazol-2-yl)ethyl]benzamideHCID 221431023-tert-Butylbenzoyl chloride

Produkt 1

HCID 20085684N-[2-(1H-Imidazol-2-yl)ethyl]-2-[[3-(1,1-dimethylethyl)-benzoyl]amino]benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21584119Ethylacetate methanolLösungsmittel

Versuchsvorschrift

The titled compound was prepared substantially in accordance with the method detailed in Example 46 using 2.50 g (0.0107 mol) of 2-amino-N-[2-(1H-imidazol-2-yl)ethyl]benzamide and 4.20 g (0.0213 mol) of meta-t-butylbenzoyl chloride with the exception that, after reducing the organic layer to dryness the resulting residue was dissolved in a 1:7 methanol/ethyl acetate solution. The resulting solution was concentrated until crystals began to form and then diethyl ether was added. The resulting solution was cooled and 2.90 g of the desired titled compound were recovered by filtration (m.p. 205°-210° C.).

Aufarbeitung

  1. concentrationThe resulting solution was concentrated until crystals
  2. customto form
  3. temperatureThe resulting solution was cooled
  4. filtration2.90 g of the desired titled compound were recovered by filtration (m.p. 205°-210° C.)

Quellen und Nachweise

ORD-Eintrag
ord-2039d2ca65f6416ba2cb7515b3eafa4d
Quelldatensatz
uspto-grants-1995_03
Patentnummer
US05397798

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