HRID2406208

反应详情

EQUATION

反应方程式

HRID 2406208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a stirred solution of benzyltributyltin (69 mg, 0.184 mmol) and 8a (19.5 mg, 0.0525 mmol) in a mixture of 2 mL of DMF and 1 mL of NEt3, was added Pd(PPh3)4 (6.0 mg, 5.3 μmol). The seal tube was sealed under argon and the mixture was stirred at 110° C. for 18 h. The reaction the mixture was cooled and concentrated to dryness in vacuo and the crude product was purified by chromatography on a silica gel column. Elution with n-heptane/EtOAc (2:1) as eluent yielded 16a as a white solid (13 mg, 65%). mp: 299° C.,

WORKUP

后处理

  1. customThe seal tube was sealed under argon
  2. customThe reaction the mixture
  3. temperaturewas cooled
  4. concentrationconcentrated to dryness in vacuo
  5. customthe crude product was purified by chromatography on a silica gel column
  6. washElution with n-heptane/EtOAc (2:1) as eluent