2,4,5-Triphenylimidazole → HCID 86751077、化合物

HRID 265355

反応式

HRID 265355 の反応式
[C:1]1([C:7]2[NH:8][C:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.BrC[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=O.[C:37](=O)([O-])[O-:38].[K+].[K+]>CC(=O)CC>[CH2:35]([O:34][C:32](=[C:37]=[O:38])[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][N:11]1[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:9]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[N:8]=[C:7]1[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH3:36]

参加物

5

反応物 3

HCID 102322,4,5-TriphenylimidazoleHCID 11430Potassium CarbonateHCID 264813Ethyl 8-bromooctanoate

生成物 1

HCID 86751077HCID 86751077、化合物収率 48.5%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 2,4,5-triphenylimidazole (11 g), ethyl 8-bromooctanoate (18.64 g), anhydrous potassium carbonate (51.3 g) and dry butanone (350 ml) was heated at reflux for 26 h. The cooled reaction mixture was filtered to remove inorganics and the filtrate was evaporated to dryness in vacuo. The residue was stirred in hexane and unreacted 2,4,5-triphenylimidazole was collected by filtration (3.1 g). The filtrate was cooled and a white precipitate was collected. Recrystallisation from hexane gave 1-(7-ethoxy-carbonyl-heptyl)-2,4,5-triphenylimidazole (8.37 g, 48.4%) as a white solid, m.p. 65°-7°.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 26 h
  3. customThe cooled reaction mixture
  4. filtrationwas filtered
  5. customto remove inorganics
  6. customthe filtrate was evaporated to dryness in vacuo
  7. filtrationunreacted 2,4,5-triphenylimidazole was collected by filtration (3.1 g)
  8. temperatureThe filtrate was cooled
  9. customa white precipitate was collected
  10. customRecrystallisation from hexane

出典と根拠

ORDレコード
ord-de315edf787b4354befe83bbfa06f099
出典データセット
uspto-grants-1997_07
特許番号
US05648373

関連ノート

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