Dimethylformamide → HCID 15462527, compound

HRID 842067Notes

Reaction equation

HRID 842067 reaction equation
[CH3:1][N:2]1[C:10](=[O:11])[NH:9][C:8]2[C:3]1=[N:4][C:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[N:6][CH:7]=2.Cl[CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>C(Cl)(Cl)Cl.O>[CH3:1][N:2]1[C:10](=[O:11])[N:9]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:8]2[C:3]1=[N:4][C:5]([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)=[N:6][CH:7]=2

Participants

7

Reactant 4

HCID 6228DimethylformamideHCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 15462514HCID 15462514, compound

Product 1

HCID 15462527HCID 15462527, compoundYield 83.3%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6212ChloroformSolvent

Procedure

A mixture of 7,9-dihydro-9-methyl-2-phenyl-8H-purin-8-one (22.6 g), ethyl chloroacetate (13.5 g), potassium carbonate (15.2 g) and dimethylformamide (250 ml) is stirred at room temperature for one hour. To the reaction mixture are added water and chloroform, and the chloroform layer is separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give crude ethyl 8,9-dihydro-9-methyl-8-oxo-2-phenyl-7H-purin-7-acetate (26 g).

Workup

  1. customthe chloroform layer is separated
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-6dd6d42fefa14b4e97f561a2ef51a116
Source dataset
uspto-grants-2002_04
Patent number
US06372740B1

Reaction notes

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