HRID2399321

反应详情

EQUATION

反应方程式

HRID 2399321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-nitro-2,2-dimethyl-3-bromomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran (0.5 g, 1.27 mmol) and methylamine (40% in water, 1.1 ml, 1.397 mmol) in methanol (12 ml) was stirred at room temperature during four hours. The solvents were evaporated under reduced pressure, and water and ethyl acetate added to the residue. After stirring, the organic phase was separated and evaporated under reduced pressure. The residue was dissolved in diethyl ether and precipitated with pentane, to give 0.31 g of 6-nitro-2,2-dimethyl-3-(methylamino)methyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran, m.p. 128° C.

WORKUP

后处理

  1. customThe solvents were evaporated under reduced pressure, and water and ethyl acetate
  2. additionadded to the residue
  3. customthe organic phase was separated
  4. customevaporated under reduced pressure
  5. dissolutionThe residue was dissolved in diethyl ether
  6. customprecipitated with pentane