HRID2172859

反应详情

EQUATION

反应方程式

HRID 2172859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl 4-(5′-chloro-3,5-dimethyl-2,4′-bipyridin-2′-yl)piperazine-1-carboxylate (5.6 g, 14 mmol) in CH2Cl2 (50 mL) was added TFA (25 mL). Then the mixture was stirred for 18 hours. TLC (CH2Cl2/MeOH=10:1) showed the starting material was consumed completely. After removal of the solvent, the residue was dissolved in CH2Cl2 (180 mL), basified with 3 N aq. NaOH until pH=11, washed with brine (40 mL), dried over Na2SO4, filtered and concentrated in vacuo to afford title compound (4.1 g, 97%) as orange oil.

WORKUP

后处理

  1. customwas consumed completely
  2. customAfter removal of the solvent
  3. dissolutionthe residue was dissolved in CH2Cl2 (180 mL)
  4. washwashed with brine (40 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo