Water → HCID 23510024, 화합물

HRID 1882903노트

반응식

HRID 1882903 반응식
CO[C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[NH:12][C:13]3[CH:19]=[C:18]([C:20]([OH:22])=[O:21])[CH:17]=[CH:16][C:14]=3[N:15]=2)=[CH:7][CH:6]=1)=[O:4].C1N=CN(C(N2C=NC=C2)=O)C=1.[CH:35]1([NH2:41])[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1.O>CN(C=O)C>[CH:35]1([NH:41][C:3]([C:5]2[CH:6]=[CH:7][C:8]([C:11]3[NH:12][C:13]4[CH:19]=[C:18]([C:20]([OH:22])=[O:21])[CH:17]=[CH:16][C:14]=4[N:15]=3)=[CH:9][CH:10]=2)=[O:4])[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1

참가 물질

6

반응물 4

HCID 962WaterHCID 7965CyclohexylamineHCID 682631,1'-CarbonyldiimidazoleHCID 160843592-[4-(Methoxycarbonyl)phenyl]-1H-benzimidazole-6-carboxylic acid

생성물 1

HCID 23510024HCID 23510024, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-(4-methoxycarbonyl-phenyl)-3H-benzoimidazole-5-carboxylic acid (5.0 g) in DMF (250 mL) and CDI (7.1 g) was stirred at RT for 3.0 hours and then treated with cyclohexyl amine (2.0 g) and refluxed for 96 hours. The reaction mixture was cooled and then poured into water (2.0 L) and stirred at RT for 16 hours. The product was filtered, washed with water and ether and then recrystallized from THF, methanol and ether. Yield 0.4 g. TLC one spot (9:1)-CH2Cl2—CH3OH.

후처리

  1. temperaturerefluxed for 96 hours
  2. temperatureThe reaction mixture was cooled
  3. stirringstirred at RT for 16 hours
  4. filtrationThe product was filtered
  5. washwashed with water and ether
  6. customrecrystallized from THF, methanol and ether

출처 및 근거

ORD 기록
ord-7013dfd498794b31b34643516c1d0a7c
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06759425B2

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