HRID2175184

反应详情

EQUATION

反应方程式

HRID 2175184 的结构方程式

PROCEDURE

实验过程

A solution of 1,4,6-trimethyl-1H-indole (800 mg, 5 mmol) in DMF (0.9 mL) was cooled to 5° C. under nitrogen. The pyrophosphoryl chloride (1.4 mL, 10 mmol) was then slowly introduced. Upon complete addition the cooling bath was removed and the reaction was allowed to warm to ambient temperature. After a total of 45 minutes the reaction was cooled to 5° C. and slowly quenched with 2N NaOH. The pH was adjusted to 8. The solid that precipitate out from the solution was collected by filtration and was washed with water. The remaining white solid was dried in the oven and was confirmed to be the title compound (875 mg, 93%).

WORKUP

后处理

  1. additionUpon complete addition the cooling bath
  2. customwas removed
  3. temperatureAfter a total of 45 minutes the reaction was cooled to 5° C.
  4. customslowly quenched with 2N NaOH
  5. filtrationThe solid that precipitate out from the solution was collected by filtration
  6. washwas washed with water
  7. customThe remaining white solid was dried in the oven