HRID846578
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
The 2-amino-3-cyanofuran produced in the preceding step was combined with 4.2 mL of triethylorthoformate, and 0.5 mL of acetic anhydride, and the mixture was heated to 130° C. for two hours. Then was added 1.8 g of sodium acetate and 3 g of 2-(4-methoxyphenyl)ethylamine, followed by 3 mL of acetic acid. The resulting mixture was heated for two hours at 130°-138° C., then cooled and diluted with water. The product was extracted with large volumes of ether. The ether extracts were combined, washed with water, dried over magnesium sulfate, and concentrated. The residue was recrystallized from ether and petroleum ether. Yield 0.65 g. M.P. 135°-136° C.
WORKUP
后处理
- temperatureThe resulting mixture was heated for two hours at 130°-138° C.
- temperaturecooled
- extractionThe product was extracted with large volumes of ether
- washwashed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue was recrystallized from ether and petroleum ether