1-Heptyl-1H-imidazole → HCID 178443957、化合物

HRID 1380355ノート

反応式

HRID 1380355 の反応式
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][CH2:13][CH2:14][O:15][S:16]([C:19]2[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=2)(=[O:18])=[O:17])=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[CH2:26]([N:33]1[CH:37]=[CH:36][N:35]=[CH:34]1)[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]>>[CH3:25][C:22]1[CH:21]=[CH:20][C:19]([S:16]([O-:18])(=[O:17])=[O:15])=[CH:24][CH:23]=1.[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([CH2:11][CH2:12][CH2:13][CH2:14][N+:35]2[CH:36]=[CH:37][N:33]([CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH:34]=2)=[CH:9][CH:10]=1)(=[O:3])[CH3:2]

参加物

3

反応物 2

HCID 1866691-Heptyl-1H-imidazoleHCID 538442024-Methylbenzenesulfonic acid 4-(4-acetylaminophenyl)butyl ester

生成物 1

HCID 178443957HCID 178443957、化合物

実験手順

Heat a mixture of 6.23 g (0.017 mole) 4-methylbenzenesulfonic acid 4-(4-acetylaminophenyl)butyl ester and 2.9 g (0.017 mole) 1-heptyl-1H-imidazole to 80° C., for 5 hours, following the reaction by thin-layer chromatography on silica gel (acetonitrile:ammonium hydroxide, 90:10). At the completion of the reaction, triturate the cooled resultant material with petroleum ether. Recrystallize the material from 25 ml hot methyl ethyl ketone with hot filtration, chill and seed to obtain the title compound.

後処理

  1. temperatureHeat
  2. customthe reaction by thin-layer chromatography on silica gel (acetonitrile:ammonium hydroxide, 90:10)
  3. customAt the completion of the reaction
  4. customtriturate the
  5. temperaturecooled resultant material with petroleum ether
  6. customRecrystallize the material from 25 ml hot methyl ethyl ketone
  7. filtrationwith hot filtration
  8. temperaturechill

出典と根拠

ORDレコード
ord-46b82c06d62d4b9483e4f339ef40c8ee
出典データセット
uspto-grants-1986_04
特許番号
US04581370

反応ノート

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