HRID1282407

反应详情

EQUATION

反应方程式

HRID 1282407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

26.1 g of the methyl 4-chloro-2-(3-methoxy-3-oxo-1-propenyl)-benzoate prepared according to Example 1 are taken up in 300 ml of methanol and transferred into an autoclave and then hydrogenated at 30° C. and a hydrogen pressure of 30 bar for 5 h, until the theoretical amount of hydrogen has been taken up. The substance contains the palladium catalyst required for the Heck coupling, so that separate addition of a hydrogenation catalyst can be dispensed with. The pressure is reduced to 1 bar, and insoluble components are then filtered off. Solvent is then removed under reduced pressure until the hydrogenation product precipitates. Recrystallization gives 21 g of methyl 4-chloro-2-(3-methoxy-3-oxo-1-propanyl)-benzoate.

WORKUP

后处理

  1. customhydrogenated at 30° C.
  2. customso that separate
  3. additionaddition of a hydrogenation catalyst
  4. filtrationare then filtered off
  5. customSolvent is then removed under reduced pressure until the hydrogenation product
  6. customprecipitates
  7. customRecrystallization