HRID638480

反应详情

EQUATION

反应方程式

HRID 638480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(2-chloro-4-trifluoromethylphenoxy)phenol (1.16 g), ethyl 4-bromo-3-methoxy-2-pentenoate (prepared in accordance with the procedure of Example 10) (1.74 g) and potassium carbonate (0.73 g) in DMF (5 ml.) is heated at about 130° for 2 hours. Thereafter, DMF is removed. The residue is filtered and washed with methylene dichloride. The filtrate is washed, dried and evaporated to dryness. The oily residue is subjected to prep. thin layer chromatography using 20% ethylacetate/hexane to yield the ethyl ester of 4-[4-(2-chloro-4-trifluoromethylphenoxy)phenoxy]-3-methoxy-2-pentenoic acid, MS m/e 444 (M+).

WORKUP

后处理

  1. temperatureis heated at about 130° for 2 hours
  2. customThereafter, DMF is removed
  3. filtrationThe residue is filtered
  4. washwashed with methylene dichloride
  5. washThe filtrate is washed
  6. customdried
  7. customevaporated to dryness