HRID353385

反应详情

EQUATION

反应方程式

HRID 353385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Part A: To a solution of the propargyl amine of Part B, Example 38 (2 g, 5.6 mmol) and powdered K2CO3 (1.9 g, 13.7 mmol) in N,N-dimethylformamide (20 mL) was added 3,5-dimethoxyphenol (2.18 g, 13.7 mmol) at ambient temperature. The resulting composition was heated to 90 degrees Celsius for 36 hours. The solution was concentrated under high vacuum and the residue was dissolved in ethyl acetate. The organic layer was washed with 1N NaOH, H2O and dried over MgSO4. Chromatography (on silica, ethyl acetate/hexane) provided phenoxy propargyl amine as light yellow gel (2.76 g, quantitative yield).

WORKUP

后处理

  1. customat ambient temperature
  2. temperatureThe resulting composition was heated to 90 degrees Celsius for 36 hours
  3. concentrationThe solution was concentrated under high vacuum
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washThe organic layer was washed with 1N NaOH, H2O
  6. dry with materialdried over MgSO4