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Dicyclohexylcarbodiimide → HCID 21909973、化合物

HRID 1245271
ノート
印刷プレビュー

反応式

HRID 1245271 の反応式
[F:1][C:2]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:13][CH:12]=2)[C:8]([F:22])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[F:23][C:24]1[CH:29]=[C:28]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[F:36])[CH:27]=[CH:26][C:25]=1O.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.ClCCl>[F:1][C:2]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:13][CH:12]=2)[C:8]([F:22])=[CH:7][C:3]=1[C:4]([O:6][C:25]1[CH:26]=[CH:27][C:28]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[F:36])=[CH:29][C:24]=1[F:23])=[O:5]
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 219099662,5-Difluoro-4-(4-pentylphenyl)benzoic acidHCID 219099682',3-Difluoro[1,1'-biphenyl]-4-ol

生成物 1

HCID 21909973HCID 21909973、化合物

試薬・触媒・溶媒 2

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

実験手順

To a mixture of 2,5-difluoro-4-(4-pentylphenyl)benzoic acid (28.40 mmol), 2-fluoro-4-(2-fluorophenyl)phenol (28.40 mmol), and dichloromethane (100 ml), 4-dimetylaminopyridine (34.10 mmol) is added dropwise. Then, a solution of 1,3-dicyclohexylcarbodiimide (34.10 mmol) in dichloromethane (100 ml) is added dropwise. After the addition is completed, the reaction mixture is stirred for 17 hrs at room temperature. Solid formed is filtered off, and a saturated aqueous solution of sodium chloride is added dropwise to the reaction mixture. The organic layer is washed with in the order of 3N-hydrochloric acid (300 ml), water, a saturated aqueous solution of sodium hydrogen carbonate (300 ml), and dried over anhydrous magnesium sulfate. The dichloromethane solution is concentrated under reduced pressure, purified by silica-gel chromatography, and further recrystallized to give the titled compound.

後処理

  1. additionis added dropwise
  2. additionAfter the addition
  3. customSolid formed
  4. filtrationis filtered off
  5. additiona saturated aqueous solution of sodium chloride is added dropwise to the reaction mixture
  6. washThe organic layer is washed with in the order of 3N-hydrochloric acid (300 ml), water
  7. dry with materiala saturated aqueous solution of sodium hydrogen carbonate (300 ml), and dried over anhydrous magnesium sulfate
  8. concentrationThe dichloromethane solution is concentrated under reduced pressure
  9. custompurified by silica-gel chromatography
  10. customfurther recrystallized

出典と根拠

ORDレコード
ord-79cc224d0cb44b61a6f1f702d90b1974
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07125589B1

反応ノート

読み込み中…

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