Water → HCID 66854185, compound

HRID 251946Notes

Reaction equation

HRID 251946 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([CH3:27])[C:5]2[N:10]=[C:9]([C:11]3[N:15]([C:16]4[C:21]([Cl:22])=[CH:20][CH:19]=[CH:18][N:17]=4)[N:14]=[C:13]([S:23][CH3:24])[CH:12]=3)[O:8][C:7](=[O:25])[C:6]=2[CH:26]=1.ClCCl.[Mg].[OH2:32]>>[Cl:1][C:2]1[CH:3]=[C:4]([CH3:27])[C:5]2[N:10]=[C:9]([C:11]3[N:15]([C:16]4[C:21]([Cl:22])=[CH:20][CH:19]=[CH:18][N:17]=4)[N:14]=[C:13]([S:23]([CH3:24])=[O:32])[CH:12]=3)[O:8][C:7](=[O:25])[C:6]=2[CH:26]=1

Participants

5

Reactant 4

HCID 962Water2×HCID 6344DichloromethaneHCID 5462224MagnesiumHCID 66854545HCID 66854545, compound

Product 1

HCID 66854185HCID 66854185, compound

Procedure

To a mixture of 0.20 g of 6-chloro-2-[1-(3-chloro-2-pyridinyl)-3-methylthio-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazine-4-one, 5 ml of dichloromethane and 0.5 ml of water was added 0.18 g of magnesium bis(monoperoxophthalate) hexahydrate (MMPP), and the resulting mixture was stirred at room temperature for 22 hours. Water was added to the reaction mixture, and the mixture was extracted with methyl t-butyl ether. The organic layer was washed with water and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 0.20 g of 6-chloro-2-[1-(3-chloro-2-pyridinyl)-3-methylsulfinyl-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazine-4-one of the formula:

Workup

  1. extractionthe mixture was extracted with methyl t-butyl ether
  2. washThe organic layer was washed with water
  3. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-0cd2baf09622477fbca57b6362b80654
Source dataset
uspto-grants-2011_01
Patent number
US07867949B2

Reaction notes

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