Potassium Carbonate → HCID 22257986, compound

HRID 1251571Notes

Reaction equation

HRID 1251571 reaction equation
Br[CH2:2][C:3]([CH3:5])=[CH2:4].C(=O)([O-])[O-].[K+].[K+].[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][C:21]2[S:32][C:24]3[NH:25][C:26](=[O:31])[N:27]([CH3:30])[C:28](=[O:29])[C:23]=3[CH:22]=2)=[CH:16][CH:15]=1>CC(C)=O.[Cl-].[Na+]>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]([CH2:20][C:21]2[S:32][C:24]3[N:25]([CH2:4][C:3]([CH3:5])=[CH2:2])[C:26](=[O:31])[N:27]([CH3:30])[C:28](=[O:29])[C:23]=3[CH:22]=2)=[CH:18][CH:19]=1

Participants

6

Reactant 3

HCID 11430Potassium CarbonateHCID 3577853-Bromo-2-methyl-1-propeneHCID 9861205HCID 9861205, compound

Product 1

HCID 22257986HCID 22257986, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 5234Sodium ChlorideSolvent

Procedure

1-Bromo-2-methyl-2-propene (0.055ml) was added to a stirred suspension of potassium carbonate (0.203 g) and 6-(4-methoxyphenylmethyl)-3-methylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (0.15 g) in acetone (5 ml). After 16 h at room temperature, the mixture was diluted with saturated aqueous sodium chloride solution and extracted with ethyl acetate. The organic extracts were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography over silica, eluting with ethyl acetate:petroleum ether (1:3 then 3:7 then 7:13) to give the title compound (0.11 g).

Workup

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography over silica
  6. washeluting with ethyl acetate:petroleum ether (1:3

Sources & evidence

ORD record
ord-7e69239051364e23b87a31e74809415e
Source dataset
uspto-grants-2002_01
Patent number
US06342502B1

Reaction notes

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