Iodoethane → (3-amino-1-ethyl-1H-pyrazol-4-yl)-phenyl-methanone

HRID 494369ノート

反応式

HRID 494369 の反応式
[NH2:1][C:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:8])=[CH:5][NH:4][N:3]=1.[H-].[Na+].[CH2:17](I)[CH3:18]>CN(C=O)C.C(OCC)(=O)C>[NH2:1][C:2]1[C:6]([C:7]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)=[O:8])=[CH:5][N:4]([CH2:17][CH3:18])[N:3]=1

参加物

6

反応物 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 178509267HCID 178509267、化合物

生成物 1

HCID 68866724(3-amino-1-ethyl-1H-pyrazol-4-yl)-phenyl-methanone

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a vigorously stirring solution of (3-amino-1H-pyrazol-4-yl)-phenyl-methanone (0.1 g, 0.53 mmol) in dry DMF at RT is added sodium hydride (0.023 g, 0.57 mmol). After 1 h, ethyl iodide (0.042 mL, 0.53 mmol) is added and stirring is continued for 4 h. The reaction mixture is diluted with ethyl acetate, washed with water, brine and dried over anhydrous sodium sulfate. The organic filtrate is concentrated and the crude is chromatographed on silica gel using 50% ethyl acetate in hexanes to provide (3-amino-1-ethyl-1H-pyrazol-4-yl)-phenyl-methanone.

後処理

  1. waitis continued for 4 h
  2. washwashed with water, brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationThe organic filtrate is concentrated
  5. customthe crude is chromatographed on silica gel using 50% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-8126096e5b3b44298db9109978e0fb0d
出典データセット
uspto-grants-2009_05
特許番号
US07538135B2

反応ノート

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