HRID1796197

反应详情

EQUATION

反应方程式

HRID 1796197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 4-(1-t-butoxycarbonylpiperidin-4-yloxy)-3-chloronitrobenzene (1.50 g) obtained in reference example 3 in 90% formic acid (4.00 g) was added 37% formaldehyde (2.50 g), and the resulting mixture was stirred at 100° C. for 2 hours. After cooling to room temperature, the reaction mixture was neutralized with an aqueous potassium carbonate solution and extracted with ethyl acetate. The extract was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated in vacuo to afford the title compound (1.12 g, yield: 98%) as a yellow solid.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated in vacuo