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Dicyclohexylcarbodiimide → HCID 19762061、化合物

HRID 248777
ノート
印刷プレビュー

反応式

HRID 248777 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[N:10][C:11]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:16][CH:15]=3)=[N:12][CH:13]=2)=[CH:4][CH:3]=1.[F:25][C:26]([CH3:33])([CH2:30][CH2:31][CH3:32])[C:27](O)=[O:28].C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[F:25][C:26]([CH3:33])([CH2:30][CH2:31][CH3:32])[C:27]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[N:10][C:11]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:16][CH:15]=3)=[N:12][CH:13]=2)=[CH:6][CH:7]=1)=[O:28]
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 6219752-(4-Butoxyphenyl)-5-(4-hydroxyphenyl)pyrimidineHCID 189241692-Fluoro-2-methylpentanoic acid

生成物 1

HCID 19762061HCID 19762061、化合物収率 15.1%

試薬・触媒・溶媒 2

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

実験手順

3.6 g (0.01 mol) of 5-(4-hydroxyphenyl)-2-(4-butyloxyphenyl)pyrimidine, 1.5 g (0.01 mol) of (-)-2-fluoro-2-methylpentanoic acid, 2.1 g (0.01 mol) of N,N'-dicylohexylcarbodiimide (DCC) and 130 mg (1.0×10-3 mol) of 4-dimethylaminopyridine were dissolved in 190 ml of dried methylene chloride, which were stirred under reflux for 6 hours. After the completion of the reaction, the precipitate was removed by filtration and then the filtrate was washed with 1 normal hydrochloric acid and further with water and thereafter dried on anhydrous magnesium sulfate. After the removal of magnesium sulfate by filtration, the filtrate was purified through a column chromatography of silica gel with a developing solvent (toluene: ethyl acetate=10:1 (V/V)) and recrystallized from 30 ml of ethanol to obtain 660 mg (yield: 15%) of a white crystal. The thus obtained compound has the aforementioned physical and chemical properties.

後処理

  1. temperatureunder reflux for 6 hours
  2. customAfter the completion of the reaction
  3. customthe precipitate was removed by filtration
  4. washthe filtrate was washed with 1 normal hydrochloric acid and further with water
  5. dry with materialdried on anhydrous magnesium sulfate
  6. customAfter the removal of magnesium sulfate
  7. filtrationby filtration
  8. customthe filtrate was purified through a column chromatography of silica gel with a developing solvent (toluene: ethyl acetate=10:1 (V/V))
  9. customrecrystallized from 30 ml of ethanol

出典と根拠

ORDレコード
ord-01fc8ba058a44009883e6279935d80d4
出典データセット
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05211879

反応ノート

読み込み中…

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