Hydrochloric Acid → HCID 14231092, compound

HRID 579733Notes

Reaction equation

HRID 579733 reaction equation
Cl[C:2]1[N:11]=[C:10]([NH2:12])[C:9]2[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1.[NH:17]1[CH2:22][CH2:21][C:20](=[O:23])[CH2:19][CH2:18]1.Cl.C(=O)([O-])[O-].[K+].[K+]>C(O)CCC>[O:23]=[C:20]1[CH2:21][CH2:22][N:17]([C:2]2[N:11]=[C:10]([NH2:12])[C:9]3[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=3)[N:3]=2)[CH2:18][CH2:19]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 337214-PiperidoneHCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamine

Product 1

HCID 14231092HCID 14231092, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A mixture of 1.0 g of 2-Chloro-4-amino-6,7-dimethoxyquinazoline, 1.28 g of 4-piperidone.HCl and 1.15 g of potassium carbonate in 50 ml of n-butanol was refluxed for 8 hours. and the solvent was removed under reduced pressure. To the residue was added 50 ml. of water and extracted with Ethyl acetate. Ethyl acetate extract was concentrated and the residue was washed with n-hexane. 0.98 g. of desired compound was obtained. mp. 228°~230° C. I.R. (KBr) 3350, 3200, 2900, 1700, 1645, 1595, 1570, 1500, 1465, 1260 cm-1 .

Workup

  1. customand the solvent was removed under reduced pressure
  2. additionTo the residue was added 50 ml
  3. extractionof water and extracted with Ethyl acetate
  4. extractionEthyl acetate extract
  5. concentrationwas concentrated
  6. washthe residue was washed with n-hexane

Sources & evidence

ORD record
ord-cd608d4e369c4f80b9516e34e11d41a4
Source dataset
uspto-grants-1988_06
Patent number
US04749705

Reaction notes

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