HRID235695

反应详情

EQUATION

反应方程式

HRID 235695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of about 19.63 g of about 50% sodium hydride in about 450 ml of dimethylformamide was added, portionwise, over about 15 minutes about 67 g of 2-phenyl-m-dioxan-5-ol. After stirring about 20 minutes, the mixture was cooled in ice and about 69.95 g of benzyl bromide was added dropwise over about 20 minutes. The mixture was stirred at room temperature overnight, water was added and the solid collected. This solid was dissolved in hot toluene, dried, filtered and diluted with an equal volume of petroleum ether. After standing about 4 hours at about 0° C. the solid was collected, giving about 90.5 g of the desired title compound.

WORKUP

后处理

  1. additionwas added
  2. temperaturethe mixture was cooled in ice
  3. stirringThe mixture was stirred at room temperature overnight
  4. customthe solid collected
  5. dissolutionThis solid was dissolved in hot toluene
  6. customdried
  7. filtrationfiltered
  8. additiondiluted with an equal volume of petroleum ether
  9. waitAfter standing about 4 hours at about 0° C.
  10. customthe solid was collected