HRID847533

反应详情

EQUATION

反应方程式

HRID 847533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 50 g of benzene was dissolved 3.05 g of methyl 5-hydroxyimino-4,5-bis(4-methoxyphenyl-3-pentenoate obtained in Example 3. Thereto was added gradually 3.91 g of N-bromosuccinimide at room temperature and the mixture was stirred at the same temperature for 2 hours. After completion of the reaction, ethyl acetate was added to the reaction mixture for dilution, and the organic layer was washed with an aqueous solution of potassium carbonate and then with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The organic layer was concentrated at a reduced pressure, and the residue was subjected to silica gel column chromatography (eluants: ethyl acetate-n-hexane) and crystallized from ether, giving the above-identified compound.

WORKUP

后处理

  1. additionwas added to the reaction mixture for dilution
  2. washthe organic layer was washed with an aqueous solution of potassium carbonate
  3. dry with materialwith a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate
  4. concentrationThe organic layer was concentrated at a reduced pressure
  5. customcrystallized from ether
  6. customgiving the above-identified compound