Potassium Carbonate → HCID 15070663, compound

HRID 357485Notes

Reaction equation

HRID 357485 reaction equation
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([O:10][CH3:11])[N:3]=1.[OH:12][CH:13]1[CH2:18][CH2:17][O:16][C:14]1=[O:15].CS([O-])=O.[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:11][O:10][C:4]1[CH:5]=[C:6]([O:8][CH3:9])[N:7]=[C:2]([O:12][CH:13]2[CH2:18][CH2:17][O:16][C:14]2=[O:15])[N:3]=1

Participants

6

Reactant 4

HCID 11430Potassium CarbonateHCID 545831alpha-Hydroxy-gamma-butyrolactoneHCID 2733271Sodium methanesulfinateHCID 51523232-Chloro-4,6-dimethoxypyrimidine

Product 1

HCID 15070663HCID 15070663, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

1.75 g (10 mmol) of 2-chloro-4,6-dimethoxypyrimidine, 1.02 g (10 mmol) of α-hydroxy-γ-butyrolactone and 0.26 g (2.5 mmol) of sodium methanesulfinate were heated in the presence of 2.07 g (15.0 mmol) of potassium carbonate in 10 ml of N,N-dimethylformamide to 120° C. with stirring. After 2 hours, the solvent was removed in a rotary evaporator at 70° C./20 mbar. The residue was taken up in 30 ml of water and 30 ml of dichloromethane. After the organic phase had been separated off, the aqueous phase was again extracted with 20 ml of dichloromethane. The combined organic phases was washed with water, dried over magnesium sulfate and evaporated. The title product was obtained in a yield of 0.43 g (15.5 percent of theory) in the form of a pale brown oil (GC content 94 percent). Other data concerning the title compound was:

Workup

  1. customthe solvent was removed in a rotary evaporator at 70° C./20 mbar
  2. customAfter the organic phase had been separated off
  3. extractionthe aqueous phase was again extracted with 20 ml of dichloromethane
  4. washThe combined organic phases was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

Sources & evidence

ORD record
ord-1c301232a08e43419a6f4cb206ccea8c
Source dataset
uspto-grants-1998_11
Patent number
US05840892

Reaction notes

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