2-Indancarboxylic Acid → 3-(2-Indanyl)carbonylamino-5-(4-methylphenyl)-pyrazole

HRID 1106615

반응식

HRID 1106615 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)[NH:4][N:3]=1.[CH2:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16][CH:15]1[C:23](O)=[O:24].Cl.CN(C)CCCN=C=NCC>N1C=CC=CC=1.C(OCC)(=O)C>[CH2:16]1[C:17]2[C:22](=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:14][CH:15]1[C:23]([NH:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)[NH:4][N:3]=1)=[O:24]

참가 물질

6

반응물 3

HCID 5757772-Indancarboxylic AcidHCID 7367685-Amino-3-(4-methylphenyl)pyrazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 117589303-(2-Indanyl)carbonylamino-5-(4-methylphenyl)-pyrazole수율 53%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

실험 절차

3-Amino-5-(4-methylphenyl)pyrazole (35 mg) and indan-2-carboxylic acid (33 mg) were dissolved in pyridine (2 ml) to which was subsequently added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (58 mg), and the mixture was stirred at room temperature overnight. The reaction solution was diluted with ethyl acetate (30 ml), washed with water (30 ml), saturated aqueous sodium bicarbonate (30 ml) and saturated brine (30 ml) and then dried over anhydrous magnesium sulfate. Then, the solvent was distilled away. The resulting crystalline residue was washed with ethyl ether to obtain the title compound (34 mg) as white crystals (melting point: 220-225° C.).

후처리

  1. washwashed with water (30 ml), saturated aqueous sodium bicarbonate (30 ml) and saturated brine (30 ml)
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThen, the solvent was distilled away
  4. washThe resulting crystalline residue was washed with ethyl ether

출처 및 근거

ORD 기록
ord-4f58320b6f424e0a9326f68d5847da3e
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06057335

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