Water → HCID 21715596, compound

HRID 1387226Notes

Reaction equation

HRID 1387226 reaction equation
[OH:1][C:2]1[C:3]([C:8]2[O:9][C:10]3[CH2:16][CH2:15][CH2:14][CH2:13][C:11]=3[N:12]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.CS([C:21]1[N:26]=[C:25]([O:27][CH3:28])[CH:24]=[C:23]([O:29][CH3:30])[N:22]=1)(=O)=O.C(=O)([O-])[O-].O>CN(C=O)C>[CH3:30][O:29][C:23]1[CH:24]=[C:25]([O:27][CH3:28])[N:26]=[C:21]([O:1][C:2]2[C:3]([C:8]3[O:9][C:10]4[CH2:16][CH2:15][CH2:14][CH2:13][C:11]=4[N:12]=3)=[N:4][CH:5]=[CH:6][CH:7]=2)[N:22]=1

Participants

6

Reactant 4

HCID 962WaterHCID 19660Carbonate IonHCID 8383634,6-Dimethoxy-2-(methylsulfonyl)pyrimidineHCID 135830839HCID 135830839, compound

Product 1

HCID 21715596HCID 21715596, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

0.12 g 2-(3-hydroxy-2-pyridyl)-4,5,6,7-tetrahydrobenzoxazole, 0.12 g 2-methanesulfonyl-4,6-dimethoxypyrimidine and 0.21 g pottasium carbonate were suspended in 3 ml DMF, and the resulting suspension was subjected to a reaction for 2 hours at 60° C. After completing the reaction, the suspension reacted was added with water and then extracted with ethyl acetate. The extract was then washed with saturated saline solution. The organic layer obtained was dried with anhydrous magnesium sulfate, and the solvent used was removed by distillation under reduced pressure. The residue obtained was purified by using silica gel column chromatography, affording the objective substance in an amount of 0.18 g.

Workup

  1. customthe resulting suspension was subjected to a reaction for 2 hours at 60° C
  2. customthe reaction
  3. customthe suspension reacted
  4. extractionextracted with ethyl acetate
  5. washThe extract was then washed with saturated saline solution
  6. customThe organic layer obtained
  7. dry with materialwas dried with anhydrous magnesium sulfate
  8. customthe solvent used was removed by distillation under reduced pressure
  9. customThe residue obtained
  10. customwas purified
  11. customaffording the objective substance in an amount of 0.18 g

Sources & evidence

ORD record
ord-7c7aa88b8f094c71a5d6ffb3a2b157ae
Source dataset
uspto-grants-2001_07
Patent number
US06268310B1

Reaction notes

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