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 2-((2-butoxycarbonylamino-3-(4-fluorophenyl)propionyl)-N-methylamino)-3-methylbutyric acid 2-(3-tert-butyl-4-hydroxyphenyl)-1-(2-pyridylcarbamoyl)ethylamide (1.67 g, 2.41 mmol) in methylene chloride (30 ml), TFA (5 ml) was added and stirred at room temperature for 1.5 hours. The reaction mixture was evaporated under reduced pressure; the thus obtained residue was mixed with chloroform, washed with a saturated aqueous NaHCO3 solution and saturated brine, dried over anhydrous magnesium sulfate and evaporated to remove the solvent under reduced pressure. The thus obtained residue was subjected to silica gel column chromatography (developing solvent: methanol:aqueous ammonia:methylene chloride=3:0.1:100), giving the titled compound (370 mg).
WORKUP
后处理
- customThe reaction mixture was evaporated under reduced pressure
- additionthe thus obtained residue was mixed with chloroform
- washwashed with a saturated aqueous NaHCO3 solution and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated
- customto remove the solvent under reduced pressure