Sodium Thiosulfate → 6-Methoxy-4-(methoxycarbonyl)methoxy-2-methylsulfonylpyrimidine

HRID 1862312노트

반응식

HRID 1862312 반응식
Cl[C:2]1C=C(C=CC=1)C(OO)=O.[CH3:12][O:13][C:14]1[N:19]=[C:18](SC)[N:17]=[C:16]([O:22][CH2:23][C:24]([O:26][CH3:27])=[O:25])[CH:15]=1.[S:28]([O-:32])([O-])(=[O:30])=S.[Na+].[Na+].C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[CH3:12][O:13][C:14]1[N:19]=[C:18]([S:28]([CH3:2])(=[O:32])=[O:30])[N:17]=[C:16]([O:22][CH2:23][C:24]([O:26][CH3:27])=[O:25])[CH:15]=1

참가 물질

6

반응물 4

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 186191496-Methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine

생성물 1

HCID 186191946-Methoxy-4-(methoxycarbonyl)methoxy-2-methylsulfonylpyrimidine

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2.59 g of 3-chloroperoxybenzoic acid was added to a solution of 1.22 g of 6-methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine in 10 ml of chloroform at 0° C. The mixture was stirred at room temperature for 3 hours, then 30 ml of saturated aqueous sodium thiosulfate solution was added to the mixture. The mixture was poured into saturated aqueous sodium bicarbonate solution, extracted with chloroform, the organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated, then, the resulted residue was subjected to silica gel chromatography to obtain 1.32 g of 6-methoxy-4-(methoxycarbonyl)methoxy-2-methylsulfonylpyrimidine.

후처리

  1. extractionextracted with chloroform
  2. washthe organic layer was washed with saturated saline
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-56687f8b62bf45dd94a4930e2edc09c4
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06537948B1

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