HRID1594007
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
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
5.33 g (15.6 mmol) of tert-butyl 4-(5-ethoxycarbonylthiazol-2-yl)piperazine-1-carboxylate [Precursor BBB60] were dissolved in ethanol together with 0.96 g (17.1 mmol) of KOH (100 ml) and stirred at 40° C. 4 h. The resulting precipitate was filtered off and dissolved in water. After this, the solution was adjusted to a pH<2 with 10% strength hydrochloric acid and extracted with chloroform. The organic phase was washed with water and a satd aq. NaCl soln and dried over MgSO4. After filtration and concentration in vacuo, 2.77 g (8.8 mmol, 56%) of tert-butyl 4-(5-carboxythiazol-2-yl)piperazine-1-carboxylate were obtained from the residue by recrystallization from diethyl ether.
WORKUP
后处理
- custom4 h
- filtrationThe resulting precipitate was filtered off
- dissolutiondissolved in water
- extractionextracted with chloroform
- washThe organic phase was washed with water
- dry with materiala satd aq. NaCl soln and dried over MgSO4
- filtrationAfter filtration and concentration in vacuo