HRID1885492

反应详情

EQUATION

反应方程式

HRID 1885492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.58 moles (536 ml) of benzyl chloroformate (95%) are added in the course of 45 minutes to 3.25 moles (500 g) of 2-amino-5-nitrophenol and 204.5 g of calcium carbonate in 1.5 liter of dioxane brought to 70° C., the temperature being maintained at between 70° C. and 80° C. When the addition is complete, heating is maintained for a further 30 minutes. The inorganic salts present in the reaction medium are removed by filtration while hot. After the addition of ice-cold water to the filtrate, the expected product crystallizes. After filtration and drying, the product obtained is recrystallized from acetic acid. It melts at 200° C.

WORKUP

后处理

  1. custombrought to 70° C.
  2. temperaturethe temperature being maintained at between 70° C. and 80° C
  3. additionWhen the addition
  4. temperatureheating
  5. temperatureis maintained for a further 30 minutes
  6. customThe inorganic salts present in the reaction medium are removed by filtration while hot
  7. additionAfter the addition of ice-cold water to the filtrate
  8. customthe expected product crystallizes
  9. filtrationAfter filtration
  10. customdrying
  11. customthe product obtained
  12. customis recrystallized from acetic acid