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Dicyclohexylcarbodiimide → HCID 67913761、化合物

HRID 846564
ノート
印刷プレビュー

反応式

HRID 846564 の反応式
[C:1]([O:16][C:17]1[CH:25]=[CH:24][C:20]([C:21]([OH:23])=[O:22])=[CH:19][CH:18]=1)(=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].O[C:27]1[CH:32]=[CH:31][C:30]([C:33]2[CH:38]=[CH:37][C:36]([C:39](=[O:48])[CH:40]([CH3:47])[CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46])=[CH:35][CH:34]=2)=[CH:29][CH:28]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.ClCCl>[C:1]([O:16][C:17]1[CH:25]=[CH:24][C:20]([C:21]([OH:23])=[O:22])=[CH:19][CH:18]=1)(=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[CH3:47][CH:40]([CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46])[C:39]([C:36]1[CH:37]=[CH:38][C:33]([C:30]2[CH:31]=[CH:32][CH:27]=[CH:28][CH:29]=2)=[CH:34][CH:35]=1)=[O:48]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 145974864-Hydroxy-4'-(2-methyloctanoyl) biphenylHCID 543778314-(Tetradecanoyloxy)benzoic acid

生成物 1

HCID 67913761HCID 67913761、化合物収率 40%

試薬・触媒・溶媒 2

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

実験手順

Into a flask were charged 96.2 mg (0.28 mmol) of 4-tetradecanoyloxy benzoic acid, 78.0 mg (0.25 mmol) of 4-hydroxy-4'-(2-methyloctanoyl) biphenyl, 63.5 mg (0.31 mmol) of dicyclohexylcarbodiimide, 3.5 mg (0.03 mmol) of 4-dimethylamino pyridine and 5 ml of dried dichloromethane, which was heated under reflux for 7 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 further with water, dried on anhydrous magnesium sulfate, and the solvent was distilled off. This product was recrystallized with ethanol to obtain 63.5 mg (yield 40%) of white 4-tetradecanoyloxy benzoic acid-4-(2-methyloctanoyl) biphenyl.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 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 and further with water
  6. dry with materialdried on anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. customThis product was recrystallized with ethanol

出典と根拠

ORDレコード
ord-efd367bae7d4482eb88eb33e8d656c24
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05137653

反応ノート

読み込み中…

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