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Benzenepropanoyl chloride → 5-Phenyl-3-(3-phenylpropionyl)aminopyrazole

HRID 567793
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인쇄 미리보기

반응식

HRID 567793 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[NH:4][N:3]=1.[C:13]1([CH2:19][CH2:20][C:21](Cl)=[O:22])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>N1C=CC=CC=1.C(OCC)(=O)C>[C:7]1([C:5]2[NH:4][N:3]=[C:2]([NH:1][C:21](=[O:22])[CH2:20][CH2:19][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH:6]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
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참가 물질

5

반응물 2

HCID 64801Benzenepropanoyl chlorideHCID 1366553-Amino-5-phenylpyrazole

생성물 1

HCID 154897545-Phenyl-3-(3-phenylpropionyl)aminopyrazole

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

실험 절차

3-Amino-5-phenylpyrazole (160 mg) was dissolved in pyridine (1 ml) to which was subsequently added 3-phenylpropionyl chloride (0.15 ml), and the mixture was stirred at room temperature for 14 hours and then at 50° C. for 30 minutes. The reaction solution was diluted with ethyl acetate (15 ml), washed with water (15 ml), 10% citric acid (15 ml), 1 N aqueous sodium hydroxide solution (15 ml) and saturated brine (15 ml) and then dried over anhydrous sodium sulfate. The solvent was distilled away under a reduced pressure, and the resulting residue was crystallized from ethanol to obtain the title compound (139 mg) as white crystals (melting point: 168 −170° C.).

후처리

  1. waitat 50° C. for 30 minutes
  2. washwashed with water (15 ml), 10% citric acid (15 ml), 1 N aqueous sodium hydroxide solution (15 ml) and saturated brine (15 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled away under a reduced pressure
  5. customthe resulting residue was crystallized from ethanol

출처 및 근거

ORD 기록
ord-f9de44c989234c88b13bca95f8b2539d
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06180653B2

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