HRID1370018

反应详情

EQUATION

反应方程式

HRID 1370018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a dry three-necked round-bottom flask equipped with nitrogen inlet and overhead stirrer was charged 3-(3-quinolyl)-2-propyn-1-ol (1 g, 5.4 mmol) in THF (10 ml) and the solution was cooled to 0° C. Potassium t-butoxide (0.67 g, 5.9 mmol) was then added followed by dicyclohexylcarbamoyl chloride (1.32 g, 5.4 mmol). The mixture was stirred for 2 hours at 0° C. and then allowed to warm up to room temperature over a period of 6 hours by which time the reaction was determined to be complete. The reaction mixture was worked up with MTBE (50 ml) and 10% NH4Cl (25 ml) and the organic layers were concentrated to an oil. The purity compared to the standard was 94% and was used as such. Yield=2 g (95%).

WORKUP

后处理

  1. customTo a dry three-necked round-bottom flask equipped with nitrogen inlet
  2. temperatureto warm up to room temperature over a period of 6 hours by which time the reaction
  3. concentrationthe organic layers were concentrated to an oil