4-Benzoyl-2-butyl-5-cyano-1-tritylimidazole → HCID 178441735、化合物

HRID 53022ノート

反応式

HRID 53022 の反応式
[C:1]([C:9]1[N:10]=[C:11]([CH2:35][CH2:36][CH2:37][CH3:38])[N:12](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[C:13]=1[C:14]#[N:15])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C>[C:1]([C:9]1[N:10]=[C:11]([CH2:35][CH2:36][CH2:37][CH3:38])[NH:12][C:13]=1[C:14]#[N:15])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

3

反応物 1

HCID 190362554-Benzoyl-2-butyl-5-cyano-1-tritylimidazole

生成物 1

HCID 178441735HCID 178441735、化合物収率 84.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

A suspension of 10.3 g of 4-benzoyl-2-butyl-5-cyano-1-tritylimidazole [prepared as described in step (i) above] in 80% v/v aqueous acetic acid was stirred at 60° C. for 5 hours. At the end of this time, the solution thus obtained was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 2:1 by volume mixture of hexane and ethyl acetate as the eluent. The resulting oily product was dissolved in carbon tetrachloride and the solution was allowed to stand at room temperature, to precipitate crystals, which were collected by filtration to give 4.46 g of the title compound, melting at 121°-122° C.

後処理

  1. customAt the end of this time, the solution thus obtained
  2. concentrationwas concentrated by evaporation under reduced pressure
  3. customthe concentrate was purified by column chromatography through silica gel
  4. additionby volume mixture of hexane and ethyl acetate as the eluent
  5. dissolutionThe resulting oily product was dissolved in carbon tetrachloride
  6. customto stand at room temperature
  7. customto precipitate crystals, which
  8. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-41c65f04e1cd470d9c1b2ead189201e9
出典データセット
uspto-grants-1997_04
特許番号
US05616599

反応ノート

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