HRID432699

反应详情

EQUATION

反应方程式

HRID 432699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under a nitrogen atmosphere, POCl3 (16.42 ml, 0.17 mol) was slowly added to a chilled (0° C.) flask containing N,N-dimethylformamide (100 ml). The resulting solution was slowly warmed to room temperature and then added dropwise to a suspension of 4-nitro-tetrazolo[1,5-a]quinolin-5-ol in N,N-dimethylformamide (300 ml). The reaction was heated to 100° C. for 30 minutes. The orange/red solution was quenched by pouring over 1 liter of ice water. A yellow precipitate formed and was collected by filtration, redissolved in chloroform (approx. 750 ml), dried (Na2SO4), filtered, and concentrated in vacuo to yield 33.74 g of 5-chloro-4-nitrotetrazolo[1,5-a]quinoline as a yellow solid.

WORKUP

后处理

  1. temperatureThe resulting solution was slowly warmed to room temperature
  2. temperatureThe reaction was heated to 100° C. for 30 minutes
  3. customThe orange/red solution was quenched
  4. additionby pouring over 1 liter of ice water
  5. customA yellow precipitate formed
  6. filtrationwas collected by filtration
  7. dissolutionredissolved in chloroform (approx. 750 ml)
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo