Ethanol → HCID 13923938, compound

HRID 570017Notes

Reaction equation

HRID 570017 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:16])[N:3]=1.[N:17]1([C:23]2[N:28]=[C:27]3[NH:29][N:30]([CH3:33])[C:31](=[O:32])[C:26]3=[CH:25][N:24]=2)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C(O)C>C(O)CC(C)C>[ClH:16].[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:20]2[CH2:19][CH2:18][N:17]([C:23]3[N:28]=[C:27]4[NH:29][N:30]([CH3:33])[C:31](=[O:32])[C:26]4=[CH:25][N:24]=3)[CH2:22][CH2:21]2)[N:3]=1

Participants

5

Reactant 3

HCID 702EthanolHCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 13769895HCID 13769895, compound

Product 1

HCID 13923938HCID 13923938, compoundYield 84%

Reagents, catalysts & solvents 1

HCID 31260Isoamyl AlcoholSolvent

Procedure

Refluxed for 5 hours in isoamyl alcohol (30 ml) were 1.74 g (7.3 mmol) of 4-amino-2-chloro-6,7-dimethoxyquinazoline and 1.60 g (7.3 mmol) of the 6-piperazino-2-methyl-3-oxo-2,3-dihydro-1H-pyrazolo[3,4-d]pyrimidine synthesized in Referential Example 82. After allowing the reaction mixture to cool down, the resultant crystals were collected by filtration and then washed with ethanol. The thus-obtained crude crystals were added with ethanol and refluxed for 2 hours. After allowing the mixture to cool down, crystals were collected by filtration and then dried to obtain 2.90 g of the above-identified compound (yield: 84%).

Workup

  1. customsynthesized in Referential Example 82
  2. temperatureto cool down
  3. filtrationthe resultant crystals were collected by filtration
  4. washwashed with ethanol
  5. customThe thus-obtained crude crystals
  6. temperaturerefluxed for 2 hours
  7. temperatureto cool down
  8. filtrationcrystals were collected by filtration
  9. customdried

Sources & evidence

ORD record
ord-7ff4d9eb5e664bd1995236c85e936b6b
Source dataset
uspto-grants-1988_03
Patent number
US04734418

Reaction notes

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