HRID432699
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting solution was slowly warmed to room temperature
- temperatureThe reaction was heated to 100° C. for 30 minutes
- customThe orange/red solution was quenched
- additionby pouring over 1 liter of ice water
- customA yellow precipitate formed
- filtrationwas collected by filtration
- dissolutionredissolved in chloroform (approx. 750 ml)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo