HRID1060018

反应详情

EQUATION

反应方程式

HRID 1060018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 4-(4-methoxypyridin-2-yl)-2-nitrobenzaldehyde (413 mg), ethyleneglycol (0.266 ml) and magnesium sulfate (1.0 g) in toluene (10 ml) was added p-toluenesulfonic acid monohydrate (334 mg), and the resultant suspension was refluxed for 5 hours. After cooling, the mixture was poured into 0.1N aqueous sodium hydroxide and extracted with ethyl acetate. The organic layer was washed with brine, dried over potassium carbonate and evaporated under reduced pressure. The residue was triturated with diisopropyl ether. The solid was collected by filtration, washed with diisopropyl ether and dried under reduced pressure to give 2-(4-(4-methoxypyridin-2-yl)-2-nitrophenyl)-1,3-dioxolane (412 mg).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over potassium carbonate
  5. customevaporated under reduced pressure
  6. customThe residue was triturated with diisopropyl ether
  7. filtrationThe solid was collected by filtration
  8. washwashed with diisopropyl ether
  9. customdried under reduced pressure