HRID426632

反应详情

EQUATION

反应方程式

HRID 426632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 200 milliliters of xylene, 11.5 grams (0.04 mole) of β,β-dichloro-α,α-difluoro-p-phenetidine.HCl and 3.6 grams (0.04 mole) of 2,6-dichlorobenzoyl isocyanate were refluxed with stirring for two hours. The xylene was thereafter removed by vacuum distillation. The residue which remained was mixed with 200 milliliters of hexane and a crystalline solid precipitated. This precipitated material was collected by suction filtration, washed with hexane and dried. The dried crude product was a light tan gummy solid melting at 160°-185° C. This crude product was purified by recrystallization from 60 milliliters of 83 percent aqueous acetic acid, leaving 85 grams of a white solid melting at 211°-213° C. (56 percent of theoretical). Nuclear magnetic resonance spectroscopy confirmed the structure as being ##STR13##

WORKUP

后处理

  1. customThe xylene was thereafter removed by vacuum distillation
  2. additionThe residue which remained was mixed with 200 milliliters of hexane
  3. customa crystalline solid precipitated
  4. filtrationThis precipitated material was collected by suction filtration
  5. washwashed with hexane
  6. customdried
  7. customThe dried crude product
  8. customThis crude product was purified by recrystallization from 60 milliliters of 83 percent aqueous acetic acid