Ethyl 4-chloroacetoacetate → HCID 178470730, 화합물

HRID 1707677노트

반응식

HRID 1707677 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178470730HCID 178470730, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bf3d7f2446e64ee0b6e07b3b1f9b9c37
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05354768

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