HRID553269

反应详情

EQUATION

反应方程式

HRID 553269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,4,6-trimethoxybenzaldehyde (20.75 g, 0.105 mol) was dissolved in dichloromethane (300 mL) and to this solution magnesium sulphate (15 g, 0.124 mol), ammonium acetate (10 g, 0.129 mol) and methyl nitroacetate (12.60 g, 0.105 mol) were added and stirred at room temperature for 2 hours. At the end of two hours, water (300 mL) was added to the reaction mass, the organic layer was separated and the aqueous layer extracted with dichloromethane (2×100 mL). The organic layers were combined and concentrated under reduced pressure to give a solid, which was crystallized from methanol (100 mL).

WORKUP

后处理

  1. additionwere added
  2. customthe organic layer was separated
  3. extractionthe aqueous layer extracted with dichloromethane (2×100 mL)
  4. concentrationconcentrated under reduced pressure
  5. customto give a solid, which
  6. customwas crystallized from methanol (100 mL)