1-Methylpiperazine → HCID 70611251, compound

HRID 47122Notes

Reaction equation

HRID 47122 reaction equation
[CH3:1][C:2]1([CH3:27])[C:11](=[O:12])[CH:10]2[C:5](=[C:6]3[N:19]=[C:18]([C:20]4[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=4)[N:17]=[C:7]3[C:8](=[O:16])[CH:9]2[CH2:13][CH2:14][Cl:15])[CH:4]=[N:3]1.[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1>>[ClH:15].[ClH:15].[ClH:15].[CH3:27][C:2]1([CH3:1])[C:11](=[O:12])[CH:10]2[C:5](=[C:6]3[N:19]=[C:18]([C:20]4[CH:21]=[CH:22][C:23]([Cl:26])=[CH:24][CH:25]=4)[N:17]=[C:7]3[C:8](=[O:16])[CH:9]2[CH2:13][CH2:14][N:32]2[CH2:33][CH2:34][N:29]([CH3:28])[CH2:30][CH2:31]2)[CH:4]=[N:3]1

Participants

3

Reactant 2

HCID 531671-MethylpiperazineHCID 706104267,7-dimethyl-2-(4-chlorophenyl)-5-(2-chloro-ethyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione

Product 1

HCID 70611251HCID 70611251, compound

Procedure

A mixture consisting of 2.1 gm of 7,7-dimethyl-2-(4-chloro-phenyl)-5-(2-chloro-ethyl)-5H,7h-imidazo[4,5-h]isoquinoline-4,6-dione and the 10 ml of N-methyl-piperazine was heated at 130° C. for 2 hours. After distilling off the excess of N-methyl-piperazine in vacuo, the residue was purified on a silicagel column (eluant: chloroform/acetone 19:1). The trihydrochloride was precipitated from acetone by addition of ethereal hydrochloric acid and recrystallized from ethanol.

Workup

  1. distillationAfter distilling off the excess of N-methyl-piperazine in vacuo
  2. customthe residue was purified on a silicagel column (eluant: chloroform/acetone 19:1)
  3. customThe trihydrochloride was precipitated from acetone by addition of ethereal hydrochloric acid
  4. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-511e17195078445faad7fd6a48d255aa
Source dataset
uspto-grants-1979_11
Patent number
US04176184

Reaction notes

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