反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To (2′-ethylaminomethyl-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid ethyl ester (44.9 g, 0.114 mol) in CH2Cl2 (450 mL) at room temperature was added triethylamine (24 mL, 0.17 mol), followed by benzylisocyanate (16.7 mL, 0.136 mol), and the reaction was stirred for 2 hours until no starting material was seen by analytical LCMS. The mixture was partitioned between H2O and CH2Cl2, and the aqueous layer was separated and extracted with CH2Cl2. The combined organic layers were dried (MgSO4) and concentrated, and the residue was purified by silica gel chromatography (0-60% EtOAc in hexanes) to give [2′-(3-benzyl-1-ethyl-ureidomethyl)-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl]-acetic acid ethyl ester.
WORKUP
后处理
- customThe mixture was partitioned between H2O and CH2Cl2
- customthe aqueous layer was separated
- extractionextracted with CH2Cl2
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated
- customthe residue was purified by silica gel chromatography (0-60% EtOAc in hexanes)