反応 #50003

反応方程式

2,4-dichloro-6-fluoro-7-nitrobenzothiazole

→

7-amino-2,4-dichloro-6-fluorobenzothiazole

溶媒

acetic acid

ethyl acetate

acetic acid

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度to reflux
3. 3
   温度The mixture was heated for 2 hours
4. 4
   温度under reflux
5. 5
   温度after cooling the mixture
6. 6
   ろ過was filtered over celite
7. 7
   その他the phases separated
8. 8
   抽出the aqueous phase extracted with ethyl acetate
9. 9
   洗浄The combined organic phases were washed with aqueous sodium hydrogen carbonate and water
10. 10
    乾燥dried with magnesium sulfate

実験手順

5 g Iron powder was added to 40 ml 5% aqueous acetic acid. The mixture was heated to reflux and a solution of 5 g 2,4-dichloro-6-fluoro-7-nitrobenzothiazole in 40 ml acetic acid and 40 ml ethyl acetate was added. The mixture was heated for 2 hours under reflux and after cooling the mixture was filtered over celite, the phases separated and the aqueous phase extracted with ethyl acetate. The combined organic phases were washed with aqueous sodium hydrogen carbonate and water and dried with magnesium sulfate. Yield: 4.3 g=97% of theory m.p.: 173° C.

出典