2-Methylpiperazine → HCID 70594839, compound

HRID 1448972Notes

Reaction equation

HRID 1448972 reaction equation
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4](Cl)[N:3]=1.[CH3:17][CH:18]1[CH2:23][NH:22][CH2:21][CH2:20][NH:19]1>C(O)CCC>[OH2:12].[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:22]2[CH2:21][CH2:20][NH:19][CH:18]([CH3:17])[CH2:23]2)[N:3]=1.[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:22]2[CH2:21][CH2:20][NH:19][CH:18]([CH3:17])[CH2:23]2)[N:3]=1

Participants

4

Reactant 2

HCID 660572-MethylpiperazineHCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamine

Product 1

HCID 70594839HCID 70594839, compoundYield 42.9%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

4-Amino-2-chloro-6,7-dimethoxyquinazoline (8.05 g.) and 2-methylpiperazine (10 g.) were heated under reflux in butanol for 15 hours. The reaction was then evaporated in vacuo and the residual oil was taken up in chloroform (200 ml.), washed with water (4×50 ml.), dried (Na2SO4) and evaporated in vacuo. The residual oil (13 g.) was recrystallized from isopropanol to give 4-amino-6,7-dimethoxy-2-(3-methylpiperazin-1-yl)quinazoline hemihydrate (3.0 g.), m.p. 185°-187° C.

Workup

  1. customThe reaction was then evaporated in vacuo
  2. washwashed with water (4×50 ml.)
  3. dry with materialdried (Na2SO4)
  4. customevaporated in vacuo
  5. customThe residual oil (13 g.) was recrystallized from isopropanol

Sources & evidence

ORD record
ord-83c6134f33dd4b0bab7d2c6162c53783
Source dataset
uspto-grants-1980_02
Patent number
US04188390

Reaction notes

Loading…