HRID1975959

反应详情

EQUATION

反应方程式

HRID 1975959 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

To a suspension of 1.05 g (4.21 mmol) 3-iodo-isonicotinic acid in 15 ml dimethoxyethane were added successively 0.243 g tetrakis(triphenylphosphine)palladium(0), 4.2 ml 2 M sodium carbonate solution in water and 0.69 g (5.05 mmol) o-tolylboronic acid. The mixture was heated under argon at 80° C. for 18 h. After cooling to room temperature the phases were separated and the organic phase was washed twice with water (pH=9). The combined aqueous layers were than adjusted to pH=3 and extracted with five portions ethyl acetate. The combined organic layers were washed with brine, dried (magnesium sulfate) and evaporated. Chromatography of the residue afforded 0.68 g (75%) of the title compound as pale yellow crystals.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the phases
  2. customwere separated
  3. washthe organic phase was washed twice with water (pH=9)
  4. extractionextracted with five portions ethyl acetate
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried (magnesium sulfate)
  7. customevaporated