HRID448557

反应详情

EQUATION

反应方程式

HRID 448557 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

A mixture of 2b (100 mg, 0.33 mmol), potassium tert-butoxide (0.1 g, 2.7 eq), 1-1 (0.35 mmol, 1.05 eq), tris(dibenzylideneacetone)dipalladium (32 mg, 0.1 eq), tri-t-butylphosphonium tetrafluoroborate (40 mg, 0.4 eq) and dioxane (1 mL) was heated at 80° C. for 18 h in a sealed vial. After allowing the reaction to cool down to room temperature, THF was added and the mixture was filtered. The filtrate was concentrated under a stream of nitrogen and the residue was taken up with 1 mL of THF and purified by preparative HPLC to afford 2-1.

WORKUP

后处理

  1. customthe reaction
  2. temperatureto cool down to room temperature
  3. filtrationthe mixture was filtered
  4. concentrationThe filtrate was concentrated under a stream of nitrogen
  5. custompurified by preparative HPLC
  6. customto afford 2-1