HRID399404

反应详情

EQUATION

反应方程式

HRID 399404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Amino-3-pyridinol N,N-diethylcarbamate (5.80 g) was refluxed for 30 minutes in 50 mL of N,N-dimethylformamide dimethyl acetal. At the end of this time the reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography (5% Et3N/ethyl acetate) to give, after concentration of the product-containing fractions, 4.63 g of chromatographically pure product. An analytically pure material was obtained by recrystallization from Et2O, m.p. 67°-69° C.

WORKUP

后处理

  1. concentrationAt the end of this time the reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by flash chromatography (5% Et3N/ethyl acetate)
  3. customto give