HRID2354072
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
- 50 °C
PROCEDURE
实验过程
A suspension of methyl-piperidin-4-yl-carbamic acid tert-butyl ester (3.57 g, 16.7 mmol), NaHCO3 (6.7 g, 79 mmol), NaI (1.5 g, 10 mmol) and 1-(2-chloro-ethyl)-3-(2,6-dimethyl-pyridin-4-yl)-urea (Example D1, 2.14 g 9.4 mmol) in THF (30 mL) is stirred at 50° C. for 14 days. The mixture is quenched with Na2CO3 (50 mL) and extracted with CH2Cl2 (5×50 mL). The organic extracts are washed with sat. aq. Na2CO3 (30 mL), dried (Na2SO4), filtered and evaporated. The residue is purified by FC to provide the title compound.
WORKUP
后处理
- customThe mixture is quenched with Na2CO3 (50 mL)
- extractionextracted with CH2Cl2 (5×50 mL)
- washThe organic extracts are washed with sat. aq. Na2CO3 (30 mL)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe residue is purified by FC