HRID1095738

反应详情

EQUATION

反应方程式

HRID 1095738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-ethylpyridin-2-amine (3.21 g, 8.19 mmol), and chloroacetaldehyde (50% aqueous solution, 2.6 ml, 10.5 mmol) in EtOH (10 ml) was refluxed vigorously for 12 hours. The reaction mixture was concentrated, and the residue was suspended in saturated aqueous sodium bicarbonate solution. The aqueous mixture was extracted with CH2Cl2 and EtOAc, and the combined organic extracts were dried over Na2SO4, filtered and concentrated to afford the desired product (1.18 g, 98% yield) as a viscous oil. MS APCI (+) m/z 147.2 (M+1) detected.

WORKUP

后处理

  1. temperaturewas refluxed vigorously for 12 hours
  2. concentrationThe reaction mixture was concentrated
  3. extractionThe aqueous mixture was extracted with CH2Cl2 and EtOAc
  4. dry with materialthe combined organic extracts were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated