HRID1018024
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
A 1-liter, four necked round bottom flask equipped with a mechanical stirrer, thermowatch, and condenser was charged with 630 grams (383 ml) of phosphorous oxychloride. The solution was heated to 50° C. and 6-methoxy-4-methyl-2-quinolone (2) (164.5 g, 0.87 moles) was added over 20 minutes. The reaction mixture was heated to reflux and held there for 2 hours. The hot reaction mixture was slowly poured into ice water (2.5 liters) and the resulting solution cooled to 30° C. The product was removed by suction filtration, washed with water and air dried to yield the title compound 156 g (86.4%); mp 144-145° C. (Lit2 mp 143.5-144.5° C.);
WORKUP
后处理
- customA 1-liter, four necked round bottom flask equipped with a mechanical stirrer
- temperatureThe reaction mixture was heated
- temperatureto reflux
- temperaturethe resulting solution cooled to 30° C
- customThe product was removed by suction filtration
- washwashed with water and air
- customdried