HRID456382

反应详情

EQUATION

反应方程式

HRID 456382 的结构方程式

PROCEDURE

实验过程

To a solution of 3-(4-hydroxy-3-methoxyphenyl)-2-propenoic acid (10 g, 51.5 mmoles) in THF (400 ml) triphenylphosphine (2.7 g, 10.3 mmoles) and carbon tetrabromide (34.16 g, 10.3 mmoles) are added and the solution is left at room temperature, under magnetic stirring, for 48 hours. The solid is filtered and then evaporated at reduced pressure. The obtained crude product is purified by chromatogrphy on silica gel eluting with n-hexane/ethyl acetate 7/3. 9 g of 3-(4-hydroxy-3-methoxyphenyl)-2-propenoic acid 4-bromobutyl ester are obtained. M.p.=86–89° C.

WORKUP

后处理

  1. filtrationThe solid is filtered
  2. customevaporated at reduced pressure
  3. customThe obtained crude product
  4. customis purified by chromatogrphy on silica gel eluting with n-hexane/ethyl acetate 7/3