Diethyl Ether → HCID 19803857, compound

HRID 1681994Notes

Reaction equation

HRID 1681994 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][N:8]2[C:14](=[O:15])[CH2:13][C:12]3[CH:16]=[C:17]([O:22][CH3:23])[C:18]([O:20][CH3:21])=[CH:19][C:11]=3[CH:10]=[CH:9]2)[CH:2]=1.[CH3:24][O:25][C:26]1[CH:27]=[C:28]([CH2:34][CH2:35][Br:36])[CH:29]=[CH:30][C:31]=1[O:32][CH3:33].C(OCC)C>CO.C(Cl)Cl>[Br-:36].[CH3:24][O:25][C:26]1[CH:27]=[C:28]([CH2:34][CH2:35][N+:1]2[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][N:8]3[C:14](=[O:15])[CH2:13][C:12]4[CH:16]=[C:17]([O:22][CH3:23])[C:18]([O:20][CH3:21])=[CH:19][C:11]=4[CH:10]=[CH:9]3)[CH:2]=2)[CH:29]=[CH:30][C:31]=1[O:32][CH3:33]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 114706023,4-Dimethoxyphenethyl bromideHCID 19803475HCID 19803475, compound

Product 1

HCID 19803857HCID 19803857, compound

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent

Conditions

Temperature
110 °C

Procedure

A mixture of 1.1 g (0.0035 mol) of 3-[(pyridin-3-yl)methyl]-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one and 2-(3,4-dimethoxyphenyl)-ethyl bromide is heated to 110° C. for 6 hours. After cooling, the reaction mixture is dissolved in a little methanol/ methylene chloride and added dropwize to 200 ml of diethylether, with vigorous stirring. The precipitate obtained is suction filtered and dried. Yield: 1.6 g (80% of theory), Melting point: 147°-150° C.

Workup

  1. temperatureAfter cooling
  2. customThe precipitate obtained
  3. filtrationfiltered
  4. customdried

Sources & evidence

ORD record
ord-16f2de8816f34fa290e98c1638caf86c
Source dataset
uspto-grants-1992_12
Patent number
US05175157

Reaction notes

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