HRID1787889

反应详情

EQUATION

反应方程式

HRID 1787889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of methyl 4-fluoro-2-hydroxybenzoate (5.1 g, 30 mmol), triphenylphosphine (9.5 g, 36 mmol), 1-tert-butoxycarbonyl-4-hydroxypiperidine (6 g, 30 mmol), and benzene (10 mL) was heated until all solids dissolved. The solution was cooled to 0° C., then sonicated while adding diethyl azodicarboxylate (6.3 g, 36 mmol) dropwise. After the addition was complete, the reaction mixture was sonicated for an additional 60 min, diluted with CH2Cl2 (25 mL), and purified by flash chromatography, eluting with 10% EtOAc in hexanes to yield the title compound (6.45 g, 61%) as a white solid.

WORKUP

后处理

  1. temperaturewas heated until all solids
  2. dissolutiondissolved
  3. customsonicated
  4. additionAfter the addition
  5. customthe reaction mixture was sonicated for an additional 60 min
  6. custompurified by flash chromatography
  7. washeluting with 10% EtOAc in hexanes