Methyl iodide → 5-Chloro-2-methylpyridazin-3(2H)-one

HRID 57850ノート

反応式

HRID 57850 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][NH:5][C:6](=[O:8])[CH:7]=1.IC.[C:11](=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[N:4][N:5]([CH3:11])[C:6](=[O:8])[CH:7]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 199057185-Chloropyridazin-3(2H)-one

生成物 1

HCID 129101445-Chloro-2-methylpyridazin-3(2H)-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-chloro-1H-pyridazin-6-one (6.000 mmol; 783.2 mg), Iodomethane (7.200 mmol; 1032 mg; 0.453 mL), and potassium carbonate (9.000 mmol; 1256 mg) in DMF (12 mL) was stirred at room temperature overnight. The mixture was filtered. The filtrate was partitioned between EtOAc and water. The organic layer was concentrated. The residue was purified on silica eluted with 0 to 40% EtOAc in DCM to afford 5-chloro-2-methyl-pyridazin-3-one as an off-white solid (514.7, 59%).

後処理

  1. filtrationThe mixture was filtered
  2. customThe filtrate was partitioned between EtOAc and water
  3. concentrationThe organic layer was concentrated
  4. customThe residue was purified on silica
  5. washeluted with 0 to 40% EtOAc in DCM

出典と根拠

ORDレコード
ord-629f6a2a648d414ab2141a7d9626c816
出典データセット
uspto-grants-2016_09
特許番号
US09434725B2

反応ノート

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