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Water → Methyl 2-chloro-4-(3-Methyl-1H-pyrazol-1-yl)benzoate

HRID 1375382
ノート
印刷プレビュー

反応式

HRID 1375382 の反応式
[Cl:1][C:2]1[CH:11]=[C:10](F)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C(=O)([O-])[O-].[K+].[K+].[CH3:19][C:20]1[CH:24]=[CH:23][NH:22][N:21]=1.O>CN1CCCC1=O>[Cl:1][C:2]1[CH:11]=[C:10]([N:22]2[CH:23]=[CH:24][C:20]([CH3:19])=[N:21]2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 2763551Methyl 2-Chloro-4-fluorobenzoateHCID 178428694HCID 178428694、化合物2 回

生成物 1

HCID 10634466Methyl 2-chloro-4-(3-Methyl-1H-pyrazol-1-yl)benzoate

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
120 °C

実験手順

20.85 g of methyl 2-chloro-4-fluorobenzoate were dissolved in 150 ml of N-methylpyrrolidone, 30.68 g of potassium carbonate and 9.38 ml of 3-methylpyrazole were added thereto, and the mixture was stirred at 120° C. for 3 hours. Additionally, thereto was added 1.79 ml of 3-methylpyrazole, and the mixture was stirred at 120° C. for 3 hours. The reaction solution was cooled, mixed with water, and extracted with EtOAc. The organic layer was washed with water and brine, and then dried over magnesium sulfate. The solvent was evaporated, and then the residue was purified by silica gel column chromatography (hexane-EtOAc (20:1)) to obtain 9.25 g of methyl 2-chloro-4-(3-metyl-1H-pyrazol-1-yl)benzoate.

後処理

  1. stirringthe mixture was stirred at 120° C. for 3 hours
  2. temperatureThe reaction solution was cooled
  3. extractionextracted with EtOAc
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated
  7. customthe residue was purified by silica gel column chromatography (hexane-EtOAc (20:1))

出典と根拠

ORDレコード
ord-561ea20210c5454e9773d7050aa0cab2
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07169772B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート