HRID1680252
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
To the above phenol (6.0 g=20 mmol) in 100 ml acetonitrile add ethyl bromoacetate (3.0 g=24 mmol) and potassium carbonate (5.4 g=39 mmol). Stir 16 hours, filter, concentrate, and partition between ether and 1.0 N HCl. Dry and concentrate the ether. Partition between 1:1 ether-hexane and 1.0 N NaOH. Acidify the aqueous layer with concentrated HCl and extract with ether. Dry and concentrate. Recrystallize from ether-hexane and dry at 0.1 mm pressure to obtain 2-[4-(hexafluoro-2-hydroxy-2-propyl)-2-methoxy-6-methylphenoxy]acetic acid, m.p. 111°-113° C.
WORKUP
后处理
- filtrationfilter
- concentrationconcentrate
- custompartition between ether and 1.0 N HCl
- customDry
- concentrationconcentrate the ether
- customPartition between 1:1 ether-hexane and 1.0 N NaOH
- extractionextract with ether
- customDry
- concentrationconcentrate
- customRecrystallize from ether-hexane
- customdry at 0.1 mm pressure