HRID1946807

反应详情

EQUATION

反应方程式

HRID 1946807 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationthe solution was concentrated under vacuum, AcOEt
  2. additionwas added
  3. washthe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. customremoved under vacuum
  6. customto afford an oily residue which
  7. customwas purified by preparative HPLC