Methyl iodide → 6-Chloro-3-methylpyrimidin-4(3H)-one

HRID 237585

반응식

HRID 237585 반응식
[Cl:1][C:2]1[N:7]=[CH:6][NH:5][C:4](=[O:8])[CH:3]=1.CI.[C:11]([O-])([O-])=O.[K+].[K+]>CC(C)=O>[Cl:1][C:2]1[N:7]=[CH:6][N:5]([CH3:11])[C:4](=[O:8])[CH:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1354454786-Chloropyrimidin-4-ol

생성물 1

HCID 43664716-Chloro-3-methylpyrimidin-4(3H)-one

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 6-chloropyrimidin-4(3H)-one (5 g), methyliodide (2.6 mL) and K2CO3 (10.6 g) in acetone (100 mL) is stirred at room temperature over night. The mixture is partitioned between water and ethyl acetate. The organic phase is washed with brine, dried (MgSO4) and concentrated. The residue is triturated with diisopropylether to give the title compound. Yield: 5.1 g; LC (method 11): tR=0.25 min; Mass spectrum (ESI+): m/z=145 [M+H]+.

후처리

  1. customThe mixture is partitioned between water and ethyl acetate
  2. washThe organic phase is washed with brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe residue is triturated with diisopropylether

출처 및 근거

ORD 기록
ord-8455eaeb5462457094da2ec384ba5b7e
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642585B2

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