HRID1680252

反应详情

EQUATION

反应方程式

HRID 1680252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationfilter
  2. concentrationconcentrate
  3. custompartition between ether and 1.0 N HCl
  4. customDry
  5. concentrationconcentrate the ether
  6. customPartition between 1:1 ether-hexane and 1.0 N NaOH
  7. extractionextract with ether
  8. customDry
  9. concentrationconcentrate
  10. customRecrystallize from ether-hexane
  11. customdry at 0.1 mm pressure