HRID1918209

反应详情

EQUATION

反应方程式

HRID 1918209 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

Palladium tetrakis-triphenylphosphine (19.3 mg, 17 μmol) was added to a degassed solution of dibromide 4 (150 mg, 334 μmol) and 4-chlorophenylboronic acid 5 (54.8 mg, 350 μmol) in ethanol: water:toluene (2:1:1, 1.67 mL) and sodium carbonate (177 mg, 1.6 mmol). The resulting mixture was heated under N2 and stirred for 1 h at 80° C. The mixture was then cooled filtered through a 0.45 μm syringe filter and concentrated under reduced pressure. Flash chromatography (ISCO system, silica, 0-50% ethyl acetate in hexane) provided 6 (76.8 mg, 48%) as a solid: LRESIMS m/z 479.8 [M+H]+, calcd. for C20H16Br1Cl1N1O4S1 480.0.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated under N2
  2. temperatureThe mixture was then cooled
  3. filtrationfiltered through a 0.45 μm syringe
  4. filtrationfilter
  5. concentrationconcentrated under reduced pressure