HRID1684279

反应详情

EQUATION

反应方程式

HRID 1684279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Dipropylamino-5-aminochroman (Example 14; 0.60 g, 2.42 mmol) was dissolved in acetic acid (10 ml) and 2,5-dimethoxytetrahydrofuran (0.40 g, 3.0 mmol) was added. The solution was refluxed for 1 hour. The solution was neutralized with NaOH (aq.) and extracted with toluene. The organic phase was dried with sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9 to give the title compound. 13C-NMR: 111.75 21.89 24.81 52.69 53.15 67.94 108.93 115.67 118.22 118.44 121.87 127.22 141.47 155.27

WORKUP

后处理

  1. temperatureThe solution was refluxed for 1 hour
  2. extractionextracted with toluene
  3. dry with materialThe organic phase was dried with sodium sulfate
  4. customevaporated to dryness
  5. customThe residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9