HRID2172859
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 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
- customwas consumed completely
- customAfter removal of the solvent
- dissolutionthe residue was dissolved in CH2Cl2 (180 mL)
- washwashed with brine (40 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo