HRID1946807
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
A solution of methyl 4-[({6-[cyclohexyl(cyclopropylmethyl)amino]pyrimidin-4-yl}carbonyl)amino]-2-fluorobenzoate (Intermediate 25, 85 mg; 0.20 mmol) in THF (5 ml) and MeOH (5 ml) was treated with an aqueous solution (5 M) of sodium hydroxide (198 μl; 0.99 mmol). After stirring for 40 hours, HCl 1 N was added until pH 3, then the solution was concentrated under vacuum, AcOEt was added and the organic layer was washed with brine, dried (MgSO4) and removed under vacuum to afford an oily residue which was purified by preparative HPLC to give the title compound as an amorphous white solid.
WORKUP
后处理
- concentrationthe solution was concentrated under vacuum, AcOEt
- additionwas added
- washthe organic layer was washed with brine
- dry with materialdried (MgSO4)
- customremoved under vacuum
- customto afford an oily residue which
- customwas purified by preparative HPLC