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

HRID 840097노트

반응식

HRID 840097 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-400fab446fab43e59e69b90e0c6b442b
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06365584B1

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