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

HRID 1862312ノート

反応式

HRID 1862312 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-56687f8b62bf45dd94a4930e2edc09c4
出典データセット
uspto-grants-2003_03
特許番号
US06537948B1

反応ノート

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