HRID1733156

反应详情

EQUATION

反应方程式

HRID 1733156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a hot, stirred solution (50° C.) of 20.0 grams of 5-chloro-4-nitrobenzotriazole in 600 milliliters of acetonitrile is added 4.2 grams of sodium hydroxide pels and 20.0 grams of isopropyl iodide. The solution is then heated to reflux for 30 hours, filtered and the solvent removed by evaporation to yield an oil. The oil is extracted with concentrated hydrochloric acid (3×200 milliliters) and the resulting solid is collected, washed with water and air dried to yield 15.0 grams (63%) of crude 5-chloro-2-isopropyl 4-nitrobenzotriazole, m.p. 67°-70° C. The analytical sample is recrystallized from n-hexane and has a m.p. 75°-76° C.

WORKUP

后处理

  1. temperatureThe solution is then heated
  2. temperatureto reflux for 30 hours
  3. filtrationfiltered
  4. customthe solvent removed by evaporation
  5. customto yield an oil
  6. extractionThe oil is extracted with concentrated hydrochloric acid (3×200 milliliters)
  7. customthe resulting solid is collected
  8. washwashed with water and air
  9. customdried