HRID1164529

反应详情

EQUATION

反应方程式

HRID 1164529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 2-oxo-5-chloro-6-bromo-3-benzothiazolineacetate (2.0 g), methanol (250 ml) and 10% sodium hydroxide aqueous solution (2.5 ml) was refluxed with stirring for 1.5 hours and then cooled with ice-water to give crystals, which were separated by filtration. The filtrate was concentrated under reduced pressure to give crystals. The combined crystals were dissolved in water (80 ml) under heating and then insoluble materials were removed by filtration. The filtrate was adjusted at pH 2-3 with 10% hydrochloric acid and cooled to give crystals, which were separated by filtration, washed with water and dried to give crystalline 2-oxo-5-chloro-6-bromo-3-benzothiazolineacetic acid (1.5 g).

WORKUP

后处理

  1. temperaturewas refluxed
  2. customto give crystals, which
  3. customwere separated by filtration
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customto give crystals
  6. temperatureunder heating
  7. custominsoluble materials were removed by filtration
  8. temperaturecooled
  9. customto give crystals, which
  10. customwere separated by filtration
  11. washwashed with water
  12. customdried