反应 #4208

ord-b9d7e217a7e7454187283988eab03121

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度while maintaining the pH at 6.5
  2. 2
    workup.WAITWhen the pH remained constant for 15 minutes
  3. 3
    其他the acetonitrile was evaporated
  4. 4
    过滤the resulting aqueous solution was filtered
  5. 5
    洗涤The precipitate was washed thoroughly with water
  6. 6
    其他to yield
  7. 7
    干燥upon drying in vacuo, 8.98 g of the title compound

实验过程

To 7.7 g (25 mmol) of 3,4-dibenzyloxyaniline in 50 ml of 1:1 acetonitrile/water at 0° C. was added chloroacetyl chloride (3.0 ml) while keeping the pH at 6.5 with saturated aqueous potassium bicarbonate. When the pH remained constant for 15 minutes, an additional 3 ml of chloroacetyl chloride was added in small portions while maintaining the pH at 6.5. When the pH remained constant for 15 minutes, the acetonitrile was evaporated, and the resulting aqueous solution was filtered. The precipitate was washed thoroughly with water to yield, upon drying in vacuo, 8.98 g of the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04723002uspto-grants-1988_02