HRID1073829

反应详情

EQUATION

反应方程式

HRID 1073829 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.205 ml of triethylamine (1,476 mmol.) and 0.133 ml of methoxyethoxymethylchloride (MEM-Cl) (1,476 mmol.) are added to a solution of 3,5-dicarboethoxy-6-methyl-2-mercaptomethyl-4-(m-nitrophenyl)-1,4-dihydropyridine (400 mg, 0,984 mmol.) in anhydrous THF. The mixture is left to react for 30' at room temperature under nitrogen atmosphere. The reaction mixture is diluted with a mixture of ethyl acetate-water 1:1 (100 ml) and the phases are separated: the organic phase is washed with a 5% sodium bicarbonate solution (3×20 ml) and water (2×20 ml), dried on sodium sulphate, filtered and the solvent is evaporated under reduced pressure, yielding 422 mg of 3,5-dicarboethoxy-6-methyl-2-(methoxyethoxy-methylthiomethyl)-4-(m-nitrophenyl)-1,4-dihydropyridine, as a glassy yellow oil.

WORKUP

后处理

  1. waitThe mixture is left
  2. customto react for 30' at room temperature under nitrogen atmosphere
  3. customthe phases are separated
  4. washthe organic phase is washed with a 5% sodium bicarbonate solution (3×20 ml) and water (2×20 ml)
  5. customdried on sodium sulphate
  6. filtrationfiltered
  7. customthe solvent is evaporated under reduced pressure