HRID2354072

反应详情

EQUATION

反应方程式

HRID 2354072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe mixture is quenched with Na2CO3 (50 mL)
  2. extractionextracted with CH2Cl2 (5×50 mL)
  3. washThe organic extracts are washed with sat. aq. Na2CO3 (30 mL)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by FC