HRID1658319

反应详情

EQUATION

反应方程式

HRID 1658319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

By the procedure of Efxample 1, a solution of p-methoxybenzyl mercaptan in dimethylsulfoxide is added slowly to a stirred suspension of sodium hydride in dry dimethylsulfoxide under nitrogen. After stirring for one hour at room temperature, 3-bromopicolinamide is added and the mixture is kept about 75°C. for three hours, then worked up by cooling, diluting with ice water, filtering off the resulting solid, washing it with water, drying and recrystallizing from aqueous dimethylformamide to give 3-(p-methoxybenzylthio)picolinamide, m.p. 252°C. (dec.).

WORKUP

后处理

  1. waitthe mixture is kept about 75°C. for three hours
  2. temperatureby cooling
  3. filtrationfiltering off the resulting solid
  4. washwashing it with water
  5. customdrying
  6. customrecrystallizing from aqueous dimethylformamide