Dicyclohexylcarbodiimide → HCID 67913779、化合物

HRID 846563ノート

反応式

HRID 846563 の反応式
[C:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)(=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].O[C:22]1[CH:27]=[CH:26][C:25]([C:28]2[CH:33]=[CH:32][C:31]([C:34](=[O:43])[CH:35]([CH3:42])[CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])=[CH:30][CH:29]=2)=[CH:24][CH:23]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.ClCCl>[C:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)(=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].[CH3:42][CH:35]([CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])[C:34]([C:31]1[CH:32]=[CH:33][C:28]([C:25]2[CH:26]=[CH:27][CH:22]=[CH:23][CH:24]=2)=[CH:29][CH:30]=1)=[O:43]

参加物

6

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 35638214-(Nonanoyloxy)benzoic acidHCID 145974864-Hydroxy-4'-(2-methyloctanoyl) biphenyl

生成物 1

HCID 67913779HCID 67913779、化合物収率 42.2%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

Into a flask were charged 80.7 mg (0.29 mmol) of 4-nonanoyloxy benzoic acid, 84.2 mg (0.27 mmol) of 4-hydroxy-4'-(2-methyloctanoyl) biphenyl, 63.5 mg (0.31 mmol) of dicyclohexylcarbodiimide, 6.0 mg (0.05 mmol) of 4-dimethylamino pyridine and 5 ml of dried dichloromethane, which was heated under reflux for 6 hours. After the cooling, the resulting solid was filtered off, and washed with dichloromethane. The organic phase was washed with 0.1 normal hydrochloric acid and then water, dried on anhydrous magnesium sulfate, and the solvent was distilled off. This product was purified by a column chromatography and recrystallized with ethanol to obtain 65.3 mg (yield 42%) of white 4-nonanoyloxy benzoic acid-4-(2-methyloctanoyl) biphenyl.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. filtrationAfter the cooling, the resulting solid was filtered off
  4. washwashed with dichloromethane
  5. washThe organic phase was washed with 0.1 normal hydrochloric acid
  6. dry with materialwater, dried on anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. customThis product was purified by a column chromatography
  9. customrecrystallized with ethanol

出典と根拠

ORDレコード
ord-48e649b6f7d34acbbd6841c22533ef8a
出典データセット
uspto-grants-1992_08
特許番号
US05137653

反応ノート

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