Dimethylformamide → 6-Methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine

HRID 1862311노트

반응식

HRID 1862311 반응식
[H-].[Na+].Cl[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[N:7]=[C:6]([S:12][CH3:13])[N:5]=1.[C:14]([O:18][CH3:19])(=[O:17])[CH2:15][OH:16].CN(C)C=O>O>[CH3:11][O:10][C:8]1[N:7]=[C:6]([S:12][CH3:13])[N:5]=[C:4]([O:16][CH2:15][C:14]([O:18][CH3:19])=[O:17])[CH:9]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 66774Methyl GlycolateHCID 98369994-Chloro-6-methoxy-2-(methylthio)pyrimidine

생성물 1

HCID 186191496-Methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine수율 59.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

0.4 g of sodium hydride was added to a mixture of 1.59 g of 4-chloro-6-methoxy-2-methylthiopyrimidine, 0.98 g of methyl glycolate and 10 ml of N,N-dimethylformamide at 0° C. The mixture was stirred at room temperature for 5 hours, then, the reaction solution was poured into water, and extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 1.22 g of 6-methoxy-4-(methoxycarbonyl)methoxy-2-methylthiopyrimidine.

후처리

  1. extractionextracted with ethyl acetate
  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-2731ef37d29f49258025de724c9914ec
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06537948B1

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