Ethyl 4-chloroacetoacetate → HCID 178470730、化合物

HRID 1707677ノート

反応式

HRID 1707677 の反応式
Cl[CH2:2][C:3](=O)[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[NH2:11][C:12]1[C:16]([CH3:17])=[C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[NH:14][N:13]=1>C(#N)C>[CH2:8]([O:7][C:5]([CH2:4][C:3]1[NH:11][C:12]2[N:13]([CH:2]=1)[N:14]=[C:15]([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[C:16]=2[CH3:17])=[O:6])[CH3:9]

参加物

4

反応物 2

HCID 69484Ethyl 4-chloroacetoacetateHCID 3184464-Methyl-5-phenyl-2H-pyrazol-3-ylamine

生成物 1

HCID 178470730HCID 178470730、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

0.78 ml of ethyl 4-chloroacetoacetate was added to a solution of 1.0 g of 3-amino-4-methyl-5-phenyl-1H-pyrazole in 25 ml of acetonitrile, and then the mixture was stirred at room temperature for 4 days. At the end of this time, the crystals which separated were filtered off and the mother liquor was concentrated by evaporation under reduced pressure. The residue was partitioned between ethyl acetate and water, and the organic phase was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography through silica gel, using a 1:1 by volume mixture of ethyl acetate and hexane as the eluent, to give 80 mg of the title compound in the form of an oil.

後処理

  1. customAt the end of this time, the crystals which separated
  2. filtrationwere filtered off
  3. concentrationthe mother liquor was concentrated by evaporation under reduced pressure
  4. customThe residue was partitioned between ethyl acetate and water
  5. washthe organic phase was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. customthe residue was purified by column chromatography through silica gel
  9. additionby volume mixture of ethyl acetate and hexane as the eluent

出典と根拠

ORDレコード
ord-bf3d7f2446e64ee0b6e07b3b1f9b9c37
出典データセット
uspto-grants-1994_10
特許番号
US05354768

反応ノート

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