HRID1691474

反应详情

EQUATION

反应方程式

HRID 1691474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of ethyl 2-hydroxy-3-methyl-2-[6-{[4-(trifluoromethoxy)phenyl]sulfonyl}-2-(trifluoromethyl)-6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepin-8-yl]butanoate (153 mg, 0.242 mmol, Example 509) in 4 mL of EtOH was added a solution of 1N LiOH (2.5 ml) in water, and the solution was stirred for 48 h at rt. LC-MS showed the reaction complete. The reaction pH was adjusted to 6-7 with 1N HCl, and the mixture was concentrated. The resulting residue was dissolved in CH2Cl2 and filtered to remove the salt. The filtrate was concentrated and the residue was purified by chromatography to give the title compound as a white solid; Mass Spectrum: m/e=606 (M+1).

WORKUP

后处理

  1. concentrationthe mixture was concentrated
  2. dissolutionThe resulting residue was dissolved in CH2Cl2
  3. filtrationfiltered
  4. customto remove the salt
  5. concentrationThe filtrate was concentrated
  6. customthe residue was purified by chromatography