HRID1527969

反应详情

EQUATION

反应方程式

HRID 1527969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Water (1 mL) and 2 M aq. sodium carbonate solution (0.39 mL, 0.78 mmol) were added at room temperature to a degassed solution of 3-(4-bromophenyl)-1-(pyridazin-4-yl)-3-o-tolylpropan-1-one (100 mg, 262 μmol), 4-boronobenzoic acid (53.8 mg, 315 μmol) and 1,1′-bis(diphenylphosphino)ferrocene-palladium(II) dichloride dichloromethane complex (11 mg, 13 μmol) in 1,4-dioxane (1.5 mL). After heating at 80° C. for 4 h the reaction mixture was partitioned between ethyl acetate and sat. aq. ammonium chloride solution. The organic layer was washed with brine, dried over magnesium sulfate, filtered, and evaporated. After chromatography (SiO2; gradient heptane/ethyl acetate 1:1 to ethyl acetate) the title compound was obtained (33 mg, 30%). Light yellow solid, MS: 423.2 [M+H]+.

WORKUP

后处理

  1. customwas partitioned between ethyl acetate and sat. aq. ammonium chloride solution
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated