HRID1579603

反应详情

EQUATION

反应方程式

HRID 1579603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

4-Hydroxy-3-mercapto-6-methyl-2-pyrone (50 g., 0.317 mole) and m-fluorobenzylchloride (45.8 g., 0.317 mole) were dissolved in pyridine (250 ml.). The temperature rose from 20° to 36°C. The resulting solution was heated at 90°C. for two hours and poured over ice and 500 ml. of concd. hydrochloric acid. This mixture was extracted with methylene chloride. The extract was dried (MgSO4) and the solvent removed by evaporation. The residue was mixed with hexane, filtered and dried, yielding 44.6 g. (53 percent) of the desired product. Recrystallization from benzene gave the pure product as a white solid, m.p. 123.5°-124°C.

WORKUP

后处理

  1. customrose from 20° to 36°C
  2. additionpoured over ice and 500 ml
  3. extractionThis mixture was extracted with methylene chloride
  4. dry with materialThe extract was dried (MgSO4)
  5. customthe solvent removed by evaporation
  6. additionThe residue was mixed with hexane
  7. filtrationfiltered
  8. customdried
  9. customyielding 44.6 g