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

HRID 237585

反応式

HRID 237585 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-8455eaeb5462457094da2ec384ba5b7e
出典データセット
uspto-grants-2014_02
特許番号
US08642585B2

関連ノート

読み込み中…