反应 #1582

反应方程式

ethyl acetate

N-(4-chloro-2-fluoro-5-nitrophenyl)-1-cyclohexene-1,2-dicarboximide

→

title product

N-(5-Amino-4-chloro-2-fluorophenyl)-1-cyclohexene-1,2-dicarboximide

溶剂

acetic acid

反应条件

后处理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   过滤filtered through diatomaceous earth
3. 3
   浓缩The filtrate is concentrated in vacuo
4. 4
   其他to obtain a dark solid
5. 5
   过滤is filtered through diatomaceous earth
6. 6
   其他the phases are separated
7. 7
   洗涤The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
8. 8
   干燥dried over anhydrous magnesium sulfate
9. 9
   浓缩concentrated in vacuo

实验过程

Iron powder (7.30 g, 130.7 mmol) is added portionwise to a mixture of N-(4-chloro-2-fluoro-5-nitrophenyl)-1-cyclohexene-1,2-dicarboximide (10.6 g, 32.7 mmol) in acetic acid (100 mL) at 65° C. After the addition is complete, the reaction mixture is stirred for 10 minutes, and filtered through diatomaceous earth. The filtrate is concentrated in vacuo to obtain a dark solid. A mixture of the solid in an ethyl acetate/saturated sodium hydrogen carbonate solution is filtered through diatomaceous earth, and the phases are separated. The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a yellow solid.

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