Water → 6-Chloro-2-cyclopropylmethyl-2H-pyridazin-3-one

HRID 80951

反応式

HRID 80951 の反応式
[CH:1]1([CH2:4]Br)[CH2:3][CH2:2]1.[Cl:6][C:7]1[CH:8]=[CH:9][C:10](=[O:13])[NH:11][N:12]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C)C=O>[Cl:6][C:7]1[CH:8]=[CH:9][C:10](=[O:13])[N:11]([CH2:4][CH:1]2[CH2:3][CH2:2]2)[N:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 2528286-Chloropyridazin-3-ol

生成物 1

HCID 581095136-Chloro-2-cyclopropylmethyl-2H-pyridazin-3-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

Cyclopropylmethyl bromide (0.82 mL) was added to a mixture of 6-chloro-2H-pyridazin-3-one (1.0 g) and K2CO3 (2.10 g) in N,N-dimethylformamide (10 mL). The resulting mixture was stirred at 60° C. overnight. Then, water was added and the mixture was extracted with ethyl acetate. The combined organic extracts were washed with water and brine and dried (MgSO4). After removal of the solvent, the residue was purified by chromatography on silica gel (CH2Cl2/MeOH/NH4OH 99:1:0.1) to afford the title compound as an oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe combined organic extracts were washed with water and brine
  3. dry with materialdried (MgSO4)
  4. customAfter removal of the solvent
  5. customthe residue was purified by chromatography on silica gel (CH2Cl2/MeOH/NH4OH 99:1:0.1)

出典と根拠

ORDレコード
ord-5c941b44a5f24da98bbb55349a3ff332
出典データセット
uspto-grants-2014_09
特許番号
US08846668B2

関連ノート

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