Dimethyl Sulfate → HCID 59803680, compound

HRID 1666220Notes

Reaction equation

HRID 1666220 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]#[C:12][C:13]2[NH:21][C:20]3[C:19](=[O:22])[NH:18][C:17](=[O:23])[N:16]([CH2:24][CH3:25])[C:15]=3[N:14]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[CH2:26](N(CC)CC)C.COS(OC)(=O)=O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]#[C:12][C:13]2[N:21]([CH3:26])[C:20]3[C:19](=[O:22])[NH:18][C:17](=[O:23])[N:16]([CH2:24][CH3:25])[C:15]=3[N:14]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Participants

5

Reactant 3

HCID 6497Dimethyl SulfateHCID 8471TriethylamineHCID 59803699HCID 59803699, compound

Product 1

HCID 59803680HCID 59803680, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a solution of 8-(3,4-dimethoxyphenylethynyl)-3-ethyl-3,7-dihydro-purine-2,6-dione (1.52 g, 4.4 mmol) in 10 ml of dimethylformamide (DMF) was added triethylamine (3 ml, 20 mmol) and dimethylsulfate (0.65 ml, 7 mmol). The mixture was stirred at room temperature for 0.5 h. The product was precipitated by addind water (40 ml), filtered under reduced pressure, washed with water and dried at 70° C. (310 mg, 20%).

Workup

  1. customThe product was precipitated by addind water (40 ml)
  2. filtrationfiltered under reduced pressure
  3. washwashed with water
  4. customdried at 70° C. (310 mg, 20%)

Sources & evidence

ORD record
ord-efd7c65a7d464e5a8bee4d67301c87d5
Source dataset
uspto-grants-2011_10
Patent number
US08044061B2

Reaction notes

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