HRID2390658

反应详情

EQUATION

反应方程式

HRID 2390658 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A suspension of Example 77A (734 mg, 1.6 mmol) and pyridyl-2-trimethylstannane (418 mg, 1.72 mmol) in DME (12 mL) was degassed with nitrogen, and PdCl2(o-tol3P)2 (62 mg, 0.078 mmol) and CuI (15 mg, 0.078 mmol) were added. The reaction vessel was sealed and the reaction was heated to 90° C. for 16 h. After cooling, the mixture was partitioned between EtOAc and H2O. The extracts were dried (Na2SO4) and concentrated, and the residue was purified by flash chromatography on silica gel, eluting with 40-75% EtOAc/hexanes to give the desired product (222 mg). MS (ESI(+)) m/e 419.0 (M+H)+.

WORKUP

后处理

  1. additionwere added
  2. customThe reaction vessel was sealed
  3. temperatureAfter cooling
  4. customthe mixture was partitioned between EtOAc and H2O
  5. dry with materialThe extracts were dried (Na2SO4)
  6. concentrationconcentrated
  7. customthe residue was purified by flash chromatography on silica gel
  8. washeluting with 40-75% EtOAc/hexanes