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Acetyl chloride → N-(2-acetyl-5-phenyl-pyrazol-3-yl)acetamide

HRID 2205796
ノート
印刷プレビュー

反応式

HRID 2205796 の反応式
[C:1]1([C:7]2[NH:11][N:10]=[C:9]([NH2:12])[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN1[CH2:19][CH2:18][O:17]CC1.[C:20](Cl)(=[O:22])[CH3:21]>C(Cl)Cl.O>[C:20]([N:10]1[C:9]([NH:12][C:18](=[O:17])[CH3:19])=[CH:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:11]1)(=[O:22])[CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6367Acetyl chlorideHCID 79724-MethylmorpholineHCID 1366553-Amino-5-phenylpyrazole

生成物 1

HCID 86717295N-(2-acetyl-5-phenyl-pyrazol-3-yl)acetamide収率 88.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 5-phenyl-1H-pyrazol-3-amine (18.6 g, 0.117 mol) and N-methylmorpholine (30.8 mL, 0.281 mol) in CH2Cl2 (250 mL) was added acetyl chloride (20 mL, 0.281 mol) dropwise at 0° C. under an atmosphere of nitrogen. The reaction mixture was stirred at room temperature for 3 h. The reaction mixture was diluted with CH2Cl2 and water. The layers were separated and the organic layer was washed with water and brine, dried (phase separator cartridge) and concentrated in vacuo. Diethyl ether was added to the residue and the solid was collected by filtration, yielding the title compound as a solid (25.1 g).

後処理

  1. customThe layers were separated
  2. washthe organic layer was washed with water and brine
  3. customdried (phase separator cartridge)
  4. concentrationconcentrated in vacuo
  5. additionDiethyl ether was added to the residue
  6. filtrationthe solid was collected by filtration

出典と根拠

ORDレコード
ord-450ce321e89f4c118f21514aeefe05b5
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09371332B2

反応ノート

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