HRID1095882
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 3-chloro-4-[2-(2-chloro-pyridin-4-yl)-3,3,3-trifluoro-2-hydroxy-1-methyl-propyl]-benzoic acid (80 mg, 0.2 mmol) and 4-amino-benzoic acid methylester (34 mg, 0.22 mmol) in N,N-dimethylformamide (4 ml) were added 4-methylmorpholine (62 mg, 0.61 mmol) and HBTU (115 mg, 0.3 mmol). The mixture was stirred for 17 h at room temperature. The reaction solution was poured in water, extracted twice with AcOEt, washed with brine, dried over MgSO4, filtered and concentrated. The residue was purified by flash chromatography (5 g silica gel, heptane/AcOEt 4:1) to give the title compound (45 mg) as a white solid. MS (m/e)=527.1 [M+H+].
WORKUP
后处理
- extractionextracted twice with AcOEt
- washwashed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by flash chromatography (5 g silica gel, heptane/AcOEt 4:1)