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

HRID 1106615ノート

反応式

HRID 1106615 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-4f58320b6f424e0a9326f68d5847da3e
出典データセット
uspto-grants-2000_05
特許番号
US06057335

反応ノート

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