Water → HCID 86701845, compound

HRID 1406028Notes

Reaction equation

HRID 1406028 reaction equation
[CH3:1][N:2]1[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:5]2[CH2:6][CH2:7][CH2:8][C:9]3[C:10](=[N:11][C:12](SC)=[N:13][CH:14]=3)[C:4]2=[N:3]1.O[O:24][S:25]([O-:27])=O.[K+].O.[CH3:30]COC(C)=O>CN(C=O)C>[CH3:1][N:2]1[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:5]2[CH2:6][CH2:7][CH2:8][C:9]3[C:10](=[N:11][C:12]([S:25]([CH3:30])(=[O:27])=[O:24])=[N:13][CH:14]=3)[C:4]2=[N:3]1

Participants

6

Reactant 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 23707502Potassium hydroxy sulfiteHCID 68295426HCID 68295426, compound

Product 1

HCID 86701845HCID 86701845, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a solution of ethyl 2-methyl-9-(methylsulfanyl)-2,4,5,6-tetrahydropyrazolo[4′,3′:6,7]cyclohepta[1,2-d]pyrimidine-3-carboxylate (100 mg, 0.31 mmol) in DMF (15 mL), oxone (580 mg, 0.94 mmol) was added. The mixture was stirred at room temperature overnight then water and AcOEt was added and the layers separated. The organic phase was finally dried over Na2SO4 and evaporated. The residue was triturated with Et2O and collected by filtration to give 105 mg (97% yield) of the title compound.

Workup

  1. customthe layers separated
  2. dry with materialThe organic phase was finally dried over Na2SO4
  3. customevaporated
  4. customThe residue was triturated with Et2O
  5. filtrationcollected by filtration

Sources & evidence

ORD record
ord-9ec8b7ba26ff43b0bdb1ca633e4d864a
Source dataset
uspto-grants-2014_12
Patent number
US08916577B2

Reaction notes

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