반응 #46806

반응 방정식

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

용매

THF

CH2Cl2

THF

반응 조건

후처리

1. 1
   세척washed with 30 mL of a saturated NaHCO3-solution
2. 2
   추출The aqueous solution was extracted with 50 mL CH2Cl2
3. 3
   건조the combined organic layers were dried over MgSO4
4. 4
   농축concentrated under reduced pressure
5. 5
   기타to give a brown solid, which

실험 절차

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.

출처