HRID1922706
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 10 mL round-bottomed flask was charged with a solution of 4-tert-butyl-3-oxopiperazine-1-carboxylic acid benzyl ester (0.75 g, 2.58 mmol) in EtOH (5 mL). The reaction mixture was flushed with nitrogen and 10% Pd/C (67 mg, 0.13 mmol) was added. The reaction mixture was stirred under a hydrogen atmosphere for 18 h. The reaction mixture was loaded onto an Isolute® SCX-2 cartridge. The cartridge was washed with MeOH and the desired product was eluted using 2 M NH3 in MeOH to give 1-tert-Butylpiperazin-2-one as grey oil (0.276 g, 69%). 1H NMR (300 MHz, CDCl3): δ 3.50 (s, 2H), 3.37 (t, J=5.5 Hz, 2H), 3.06 (t, J=5.5 Hz, 2H), 1.48-1.41 (m, 9H)
WORKUP
后处理
- additionwas added
- washThe cartridge was washed with MeOH
- washthe desired product was eluted