HRID1441726

反应详情

EQUATION

反应方程式

HRID 1441726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

2-Fluoro-4-nitrobenzaldehyde (1.00 g, 5.92 mmol) and acetamidine hydrochloride (0.783 g, 8.28 mmol) were added to a suspension of activated 4 Å MS (1.2 g) in acetonitrile (60 mL). K2CO3 (1.14 g, 8.28 mmol) was then added and the reaction was heated to reflux for 4 h. The reaction was then cooled to 25° C. and filtered through celite rinsing with CH2Cl2. The crude product was purified by flash chromatography on silica eluting with 0-10% acetone in CH2Cl2 to give 0.386 g of compound 25A as a yellow solid.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 4 h
  3. filtrationfiltered
  4. washthrough celite rinsing with CH2Cl2
  5. customThe crude product was purified by flash chromatography on silica eluting with 0-10% acetone in CH2Cl2