HRID1828376

反应详情

EQUATION

反应方程式

HRID 1828376 的结构方程式

CONDITIONS

反应条件

温度
4 °C

PROCEDURE

实验过程

Diaminopicric acid (0.100 g, 0.386 mmol) is suspended in water (6.85 ml) and a 50% aqueous solution of sodium hydroxide (0.65 ml,12.5 mmol) is added. The suspension is stirred for 0.5 hr in a heated water bath (98–100° C.) to produce an orange-red suspension which is cooled to 4° C. Addition of cold 12N hydrochloric acid (4 ml) produces a deep yellow suspension that is heated to solution. Cooling to 4° C. produces orange-yellow crystals (needles) that are collected, washed with cold 3N hydrochloric acid and dried to give trinitrophloroglucinol (0.085 g) in 84% yield. The IR spectrum for this material corresponds to that for known trinitrophloroglucinol.

WORKUP

后处理

  1. customto produce an orange-red suspension which
  2. customproduces a deep yellow suspension that
  3. temperatureis heated to solution
  4. temperatureCooling to 4° C.
  5. customproduces orange-yellow crystals (needles) that
  6. customare collected
  7. washwashed with cold 3N hydrochloric acid
  8. customdried