HRID66015
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 25.2 g. of sodium bicarbonate, 12.3 g. of 2-aminopyridine and 30 g. of α-bromo-p-methoxyacetophenone in 100 ml. of water and 550 ml. of absolute ethanol is heated at reflux temperatures for 1.5 hrs. The reaction mixture is concentrated under reduced pressure to a yellow solid, which is partitioned between chloroform and water. The organic layer is separated, dried over sodium sulfate. Removal of the chloroform in vacuo leaves the crude intermediate as a yellow solid. Recrystallization from ethanolwater give 15.2 g. of the desired material, m.p. 131-134° C.
WORKUP
后处理
- additionA mixture of 25.2 g
- temperatureat reflux temperatures for 1.5 hrs
- concentrationThe reaction mixture is concentrated under reduced pressure to a yellow solid, which
- customis partitioned between chloroform and water
- customThe organic layer is separated
- dry with materialdried over sodium sulfate
- customRemoval of the chloroform in vacuo