HRID361325

反应详情

EQUATION

反应方程式

HRID 361325 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-amino-3-pyridinol (3.90 g), N,N-diethylformamide dimethyl acetal (11.68 g) and toluene (20 mL) was heated under nitrogen for 2 hours. The solution was concentrated under reduced pressure. The resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran to give a solid. Recrystallization of the purified product from ethyl acetate/hexanes afforded 4.21 g of crystalline solid, m.p. 104°-106° C.

WORKUP

后处理

  1. temperaturewas heated under nitrogen for 2 hours
  2. concentrationThe solution was concentrated under reduced pressure
  3. filtrationThe resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran
  4. customto give a solid
  5. customRecrystallization of the purified product from ethyl acetate/hexanes