反応 #46806

反応方程式

4-(4-amino-phenyl)-morpholin-3-one

NaHCO3

H2O

methyl-2-trichloromethyl-1H-benzoimidazole-4-carboxylate

→

2-[4-(3-Oxo-morpholin-4-yl)-phenylcarbamoyl]-1H-benzoimidazole-4-carboxylic acid methyl ester

溶媒

THF

CH2Cl2

THF

反応条件

後処理

1. 1
   洗浄washed with 30 mL of a saturated NaHCO3-solution
2. 2
   抽出The aqueous solution was extracted with 50 mL CH2Cl2
3. 3
   乾燥the combined organic layers were dried over MgSO4
4. 4
   濃縮concentrated under reduced pressure
5. 5
   その他to give a brown solid, which

実験手順

A solution of 69.4 mg (0.236 mmol) methyl-2-trichloromethyl-1H-benzoimidazole-4-carboxylate in 2 mL THF were slowly added to a mixture containing 50 mg (0.26 mmol) 4-(4-amino-phenyl)-morpholin-3-one, 220 mg (2.62 mmol) NaHCO3, 8 mL THF and 3 mL H2O. The mixture was stirred vigorously for 3 h at room temperature, diluted with 50 mL CH2Cl2 and washed with 30 mL of a saturated NaHCO3-solution. The aqueous solution was extracted with 50 mL CH2Cl2 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.

出典