Methyl iodide → 6-Chloro-2-methyl-2,3-dihydropyridazin-3-one

HRID 919293

反応式

HRID 919293 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5](=[O:8])[NH:6][N:7]=1.[C:9]([O-])([O-])=O.[K+].[K+].CI>C(#N)C.CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5](=[O:8])[N:6]([CH3:9])[N:7]=1

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 2528286-Chloropyridazin-3-ol

生成物 1

HCID 27836076-Chloro-2-methyl-2,3-dihydropyridazin-3-one

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution 6-chloropyridazin-3(2H)-one (130 mg, 1.0 mmol) in acetonitrile (3.0 mL) was added K2CO3 (437 mg, 3.16 mmol), CH3I (299 mg, 2.11 mmol), the reaction mixture was stirred at reflux for 2 h. The mixture was cooled to ambient temperature, diluted with EtOAc (20 mL), washed with sodium bicarbonate (10 mL) and brine (10 mL), dried over MgSO4, filtered and concentrated. The residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1) to obtained product: LC/MS m/z=145 (M+H)+.

後処理

  1. temperatureat reflux for 2 h
  2. washwashed with sodium bicarbonate (10 mL) and brine (10 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1)
  7. customto obtained product

出典と根拠

ORDレコード
ord-8a9f4b1f7eea4bc698fd87d0c961aa8d
出典データセット
uspto-grants-2016_03
特許番号
US09273033B2

関連ノート

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