HRID719639

反应详情

EQUATION

反应方程式

HRID 719639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

2-Chloro-5-iodo-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (5.00 g, Example 14a), tetrabutylammonium chloride (3.40 g) and sodium hydrogencarbonate (2.44 g) were charged to a flask. Pd(OAc)2 (0.0533 g), toluene (50 ml) and allyl alcohol (1.01 ml) were added to afford a pale brown mixture which was heated at 80° C. for 5 h. The resulting dark brown mixture was cooled to ambient then filtered to remove the solid residues. These were washed with further toluene (2×50 ml) and the combined toluene extracts then washed with water (100 ml), dried over MgSO4 and concentrated to a light brown solid (3.82 g).

WORKUP

后处理

  1. customto afford a pale brown mixture which
  2. temperatureThe resulting dark brown mixture was cooled
  3. filtrationto ambient then filtered
  4. customto remove the solid residues
  5. washThese were washed with further toluene (2×50 ml)
  6. washthe combined toluene extracts then washed with water (100 ml)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated to a light brown solid (3.82 g)