反応 #76505

反応方程式

product

1,4,7,8,9,10-Hexahydro-9-methyl-pyrido-[3,4-f]quinoxaline-2,3-dione monohydrochloride

potassium nitrate

sulfuric acid

sulfuric acid

ammonium hydroxide

→

title compound

収率 100.0%

1,4,7,8,9,10-Hexahydro-9-methyl-6-nitro-pyrido-[3.4-f]quinoxaline-2,3-dione methansulfonate

収率 100.0%

反応条件

後処理

1. 1
   workup.ADDITIONwas poured onto ice
2. 2
   温度cooled in a dry ice bath
3. 3
   ろ過The orange/yellow solid was collected by filtration
4. 4
   洗浄washed consecutively with water, acetone and ether
5. 5
   その他dried

実験手順

A solution of the product from Example 77 (0.64 g, 2.77 mmol) in 20 mL concentrated sulfuric acid was treated with potassium nitrate (0.29 g, 2.87 mmol) in 2 mL concentrated sulfuric acid. After stirring overnight at room temperature the reaction mixture was poured onto ice, cooled in a dry ice bath, and then basified with ammonium hydroxide to pH 8.9. The orange/yellow solid was collected by filtration and washed consecutively with water, acetone and ether and dried to give the title compound (0.78 g, 100% yield).

出典