Dimethylamine → HCID 13225518, compound

HRID 464524Notes

Reaction equation

HRID 464524 reaction equation
Cl[C:2]1[N:3]=[CH:4][C:5]2[CH2:6][N:7]=[C:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[C:9]3[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:10]=3[C:11]=2[N:12]=1.[CH3:25][NH:26][CH3:27]>CN(C)C=O>[Cl:17][C:15]1[CH:14]=[CH:13][C:10]2[C:11]3[N:12]=[C:2]([N:26]([CH3:27])[CH3:25])[N:3]=[CH:4][C:5]=3[CH2:6][N:7]=[C:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[C:9]=2[CH:16]=1

Participants

4

Reactant 2

HCID 674DimethylamineHCID 13225515HCID 13225515, compound

Product 1

HCID 13225518HCID 13225518, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A solution of 4.0 g (0.0112 mol) of 2,9-dichloro-7-(2-fluorophenyl)-5H-pyrimido[5,4-d][2]benzazepine in 15 ml of N,N-dimethylformamide was cooled in an ice bath and saturated with dimethylamine. After 18 hr at room temperature, 80 ml of ice water was added and the precipitate was collected by filtration and recrystallized twice from methanol to give the end product as white rods, mp 175°-179°.

Workup

  1. filtrationthe precipitate was collected by filtration
  2. customrecrystallized twice from methanol
  3. customto give the end product as white rods, mp 175°-179°

Sources & evidence

ORD record
ord-7ac29f8cdb5446dc8f5e2d34407b7280
Source dataset
uspto-grants-1985_10
Patent number
US04547581

Reaction notes

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