Tetrahydrofuran → HCID 18425438, compound

HRID 1280592Notes

Reaction equation

HRID 1280592 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13](SC)=[N:14][CH:15]=2)[N:10]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:9]1=[O:26].O[O:28][S:29]([O-:31])=O.[K+].O1CCC[CH2:34]1>O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([S:29]([CH3:34])(=[O:31])=[O:28])=[N:14][CH:15]=2)[N:10]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:9]1=[O:26]

Participants

6

Reactant 3

HCID 8028TetrahydrofuranHCID 184254393-(2-chlorophenyl)-7-methylthio-1-phenyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-oneHCID 23707502Potassium hydroxy sulfite

Product 1

HCID 18425438HCID 18425438, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8857Ethyl AcetateSolvent

Procedure

To 3-(2-chlorophenyl)-7-methylthio-1-phenyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (2 g) in 20 mL of tetrahydrofuran at 0° C. was added a solution of 8.1 g of Oxone® in 24 mL of water. The mixture was stirred for 5 hours at room temperature, diluted with ethyl acetate, washed with brine, dried over sodium sulfate, filtered, and evaporated to give 2 g of 3-(2-chlorophenyl)-7-methanesulfonyl-1-phenyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one, m.p. 185.8-186.3° C.

Workup

  1. washwashed with brine
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated

Sources & evidence

ORD record
ord-3eaf2b2d36c3460c908287efb4adb424
Source dataset
uspto-grants-2002_09
Patent number
US06451804B1

Reaction notes

Loading…