HRID259253
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 2- acetylbenzoic acid (6.21g), diethyl bromomalonate (9.0g.) and potassium hydroxide (2.12g.) in ethanol (50ml.) was heated under reflux for 6 hours. The cooled mixture was evaporated to dryness, water (100ml.) added and extracted with ether. The combined ethereal extracts were washed with water, dried and evaporated to dryness. The residue was heated under reflux with a mixture of concentrated hydrochloric acid (160ml.) -- acetic acid (100ml.) for two hours, cooled poured into iced water (1 liter). Filtration gave the product as a white solid, mp. 250° -2°, (lit mp. 248° -9°) (Found: C, 64.59; H, 4.01. C11H8O4 requires C, 64.70; H, 3.95).
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 6 hours
- customThe cooled mixture was evaporated to dryness, water (100ml.)
- additionadded
- extractionextracted with ether
- washThe combined ethereal extracts were washed with water
- customdried
- customevaporated to dryness
- temperatureThe residue was heated
- temperatureunder reflux with a mixture of concentrated hydrochloric acid (160ml.)
- temperaturecooled
- additionpoured into iced water (1 liter)
- filtrationFiltration