HRID1600448

反应详情

EQUATION

反应方程式

HRID 1600448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 50.0 g (0.400 mol) of nicotinic acid, 50.0 g (0.400 mol) of methyl glycinate hydrochloride, 90 g (0.440 mol) of dicyclohexylcarbodiimide, and 2 g of p-toluenesulfonic acid in 500 ml of dry pyridine was stirred overnight at room temperature. Filtration and evaporation in vacuo gave a heavy oil which was dissolved in 500 ml of water. After basification with ammonia the aqueous solution was extracted with 3×300 ml of dichloromethane. The organic phase was dried over magnesium sulphate, and removal of the solvent in vacuo gave crude 77 as a heavy yellow oil. Yield: 63.0 g (0.320 mol, 81%).

WORKUP

后处理

  1. filtrationFiltration and evaporation in vacuo
  2. customgave a heavy oil which
  3. extractionAfter basification with ammonia the aqueous solution was extracted with 3×300 ml of dichloromethane
  4. dry with materialThe organic phase was dried over magnesium sulphate, and removal of the solvent in vacuo