Chloride → 6-Amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine

HRID 1836197

반응식

HRID 1836197 반응식
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[NH:5][C:4](=O)[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[Cl-].[C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25]Br)(=[O:20])[CH3:19]>CC(C)=O>[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[N:5]=[C:4]([CH2:25][CH2:24][CH2:23][CH2:22][O:21][C:18](=[O:20])[CH3:19])[CH:3]=1

참가 물질

6

반응물 4

HCID 312ChlorideHCID 11430Potassium CarbonateHCID 784911-Butanol, 4-bromo-, 1-acetateHCID 1354042146-Amino-2-methoxy-3,4-dihydropyrimidin-4-one

생성물 1

HCID 234990886-Amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine수율 42%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Alternative Method B. A mixture of 6-amino-2-methoxy-4-pyrimidone (30 g, 212.6 mmol), K2CO3 (44 g, 318 mmol), benzyltriethylammionium chloride (20 g, 88 mmol) and 4-bromobutyl acetate (60 g, 308 mmol) in acetone (800 ml) was heated at reflux overnight. After cooling to room temperature, the insoluble salts were filtered off and the solvent was removed. The residue was purified by chromatography on silica gel with CHCl3/MeOH (100:2-100:5) as eluent. After separation of 6-amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine (22.8, yield 42%), 18.7 g (yield 34.5%) of 6-amino-2-methoxy-3-(4-acetoxybutyl)-4-pyrimidone was isolated as a white solid.

후처리

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. filtrationthe insoluble salts were filtered off
  4. customthe solvent was removed
  5. customThe residue was purified by chromatography on silica gel with CHCl3/MeOH (100:2-100:5) as eluent

출처 및 근거

ORD 기록
ord-c02c628edb0048c4a13daa4ec2f86a16
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06777420B2

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