HRID1055646

反应详情

EQUATION

反应方程式

HRID 1055646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

200 mg (0.61 mmol) of the compound of Example 15A were dissolved in 2.0 ml of DMF, and the mixture was degassed with argon. After addition of 79 mg (0.67 mmol) of zinc cyanide and 42 mg (0.04 mmol) of tetrakis(triphenylphosphine)palladium(0), the reaction was stirred in a microwave oven (Biotage Initiator, with Dynamic Field Tuning) at 120° C. for 30 min. After cooling, solid components were filtered off and the filtrate was separated into its components by preparative HPLC (Method 15). Concentration of the product fractions and drying of the residue under high vacuum gave 115 mg (88% pure, 61% of theory) of the title compound.

WORKUP

后处理

  1. customthe mixture was degassed with argon
  2. temperatureAfter cooling
  3. filtrationsolid components were filtered off
  4. customthe filtrate was separated into its components by preparative HPLC (Method 15)
  5. customConcentration of the product fractions and drying of the residue under high vacuum