Water → HCID 23510024、化合物

HRID 1882903ノート

反応式

HRID 1882903 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 23510024HCID 23510024、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7013dfd498794b31b34643516c1d0a7c
出典データセット
uspto-grants-2004_07
特許番号
US06759425B2

反応ノート

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