HRID361325
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated under nitrogen for 2 hours
- concentrationThe solution was concentrated under reduced pressure
- filtrationThe resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran
- customto give a solid
- customRecrystallization of the purified product from ethyl acetate/hexanes