4-Benzoyl-2-butyl-5-cyano-1-tritylimidazole → HCID 178441735, 화합물

HRID 53022노트

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HRID 53022 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

HCID 178441735HCID 178441735, 화합물수율 84.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-41c65f04e1cd470d9c1b2ead189201e9
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616599

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