HRID343269

反应详情

EQUATION

反应方程式

HRID 343269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12 g nifedipine was placed in a 100-mL three-neck flask and dissolved in 50 mL tetrahydrofuran under nitrogen. To this was added 1.66 g of an oil dispersion of sodium hydride (60% NaH) with stirring. After stirring for a brief period of time, 10 mL methyl iodide was added and the reaction was stirred for 1 hour at 38° C. 200 mL ethyl acetate was then added and the organic layer was washed several times with water and dried over sodium sulfate. The sodium sulfate was filtered off and the solvent was removed from the filtrate on a rotary evaporator. The resulting solid was dissolved in 200 mL MIBK. The addition of hexane gave 8.9 g N-methylnifedipine as yellow crystals.

WORKUP

后处理

  1. additionwas added
  2. stirringthe reaction was stirred for 1 hour at 38° C
  3. washthe organic layer was washed several times with water
  4. dry with materialdried over sodium sulfate
  5. filtrationThe sodium sulfate was filtered off
  6. customthe solvent was removed from the filtrate on a rotary evaporator
  7. dissolutionThe resulting solid was dissolved in 200 mL MIBK
  8. additionThe addition of hexane