Diethylether ethylacetate → N-{2-[2-(4-Cyanophenyl)-ethyl]-1-(3,5-bis-trifluoromethyl-benzyl)-benzimidazol-5-yl}-benzenesulphonamide

HRID 840097ノート

反応式

HRID 840097 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([NH:24][S:25]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)(=[O:27])=[O:26])[CH:5]=[CH:6][C:7]=1[NH:8][CH2:9][C:10]1[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[C:12]([C:20]([F:23])([F:22])[F:21])[CH:11]=1.[C:34]([C:36]1[CH:41]=[CH:40][C:39]([CH:42]([CH3:46])C(O)=O)=[CH:38][CH:37]=1)#[N:35].[C:47](OCC)(=O)C.C(OCC)C>O=P(Cl)(Cl)Cl>[C:34]([C:36]1[CH:37]=[CH:38][C:39]([CH2:42][CH2:46][C:47]2[N:8]([CH2:9][C:10]3[CH:15]=[C:14]([C:16]([F:19])([F:17])[F:18])[CH:13]=[C:12]([C:20]([F:21])([F:22])[F:23])[CH:11]=3)[C:7]3[CH:6]=[CH:5][C:4]([NH:24][S:25]([C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)(=[O:26])=[O:27])=[CH:3][C:2]=3[N:1]=2)=[CH:40][CH:41]=1)#[N:35]

参加物

5

反応物 3

HCID 21584169Diethylether ethylacetateHCID 225698632-(4-Cyanophenyl)propanoic acidHCID 22621789n-{3-Amino-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide

生成物 1

HCID 22621791N-{2-[2-(4-Cyanophenyl)-ethyl]-1-(3,5-bis-trifluoromethyl-benzyl)-benzimidazol-5-yl}-benzenesulphonamide

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

反応条件

温度
110 °C

実験手順

N-{3-amino-4-(3,5-bis-trifluoromethyl-benzylamino)-phenyl}-benzenesulphonamide (5.5 g, 11.2 mmol) and p-cyano-phenylpropionic acid (2.35 g, 13.4 mmol) are taken up in 50 mL POCl3, and stirred for 2 h at 100-120° C. A precipitate settles out from the initially clear solution in the course of the reaction. After cooling it is diluted with 100 mL ethyl acetate/diethylether=1/1. The crystals are filtered off and washed with diethylether.

後処理

  1. customA precipitate settles out from the initially clear solution in the course of the reaction
  2. temperatureAfter cooling it
  3. filtrationThe crystals are filtered off
  4. washwashed with diethylether

出典と根拠

ORDレコード
ord-400fab446fab43e59e69b90e0c6b442b
出典データセット
uspto-grants-2002_04
特許番号
US06365584B1

反応ノート

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