Water → 1H-Benzoimidazole-2-carboxylic acid [4-(4-oxo-4H-pyridin-1-yl)-phenyl]-amide

HRID 18533

反応式

HRID 18533 の反応式
Cl[C:2](Cl)(Cl)[C:3]1[NH:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[N:4]=1.[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([N:21]2[CH:26]=[CH:25][C:24](=[O:27])[CH:23]=[CH:22]2)=[CH:17][CH:16]=1.C([O-])(O)=[O:29].[Na+].O>C1COCC1.C(Cl)Cl>[O:27]=[C:24]1[CH:23]=[CH:22][N:21]([C:18]2[CH:19]=[CH:20][C:15]([NH:14][C:2]([C:3]3[NH:7][C:6]4[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=4[N:4]=3)=[O:29])=[CH:16][CH:17]=2)[CH:26]=[CH:25]1

参加物

7

反応物 4

HCID 962WaterHCID 77133Benzimidazole, 2-trichloromethyl-HCID 516892Sodium BicarbonateHCID 574375331-(4-Amino-phenyl)-1H-pyridin-4-one

生成物 1

HCID 867611321H-Benzoimidazole-2-carboxylic acid [4-(4-oxo-4H-pyridin-1-yl)-phenyl]-amide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 769 mg 2-Trichloromethyl-1H-benzoimidazole in 10 mL THF were slowly added to a mixture containing 304 mg 1-(4-Amino-phenyl)-1H-pyridin-4-one, 1.3 g NaHCO3, 40 mL THF and 15 mL H2O. The mixture was stirred vigorously for 3 h at room temperature, diluted with 200 mL CH2Cl2 and washed with 40 mL of a saturated NaHCO3-solution. The aqueous solution was extracted with CH2Cl2 (3×200 ml) and the combined organic layers were dried over MgSO4 and concentrated under reduced pressure to give a brown solid, which was pure enough for the following reactions.

後処理

  1. washwashed with 40 mL of a saturated NaHCO3-solution
  2. extractionThe aqueous solution was extracted with CH2Cl2 (3×200 ml)
  3. dry with materialthe combined organic layers were dried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customto give a brown solid, which

出典と根拠

ORDレコード
ord-ce1eae390e274e7aaf0ec5c11672db47
出典データセット
uspto-grants-2010_06
特許番号
US07741341B2

関連ノート

読み込み中…