反応 #1138118

反応方程式

potassium formate

N-{3-[(2-chloro-5-methoxyphenyl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamide

THF

water

→

3-amino-N-{3-[(2-chloro-5-methoxyphenyl)amino]quinoxalin-2-yl}benzenesulfonamide hydrochloride

溶媒

methanol

ethanol

反応条件

後処理

1. 1
   温度heated to reflux
2. 2
   workup.STIRRINGThe reaction mixture is stirred
3. 3
   温度at reflux until completion of the reaction
4. 4
   workup.STIRRINGa one hour stirring
5. 5
   ろ過the catalyst is filtered off
6. 6
   洗浄washed with 3.4 volumes of methanol
7. 7
   温度The filtered solution is cooled down at 20° C
8. 8
   workup.ADDITION0.62 kg of HCl are added
9. 9
   workup.STIRRINGThe reaction mixture is stirred at 20° C.
10. 10
    温度cooled down at 5° C.
11. 11
    ろ過filtered
12. 12
    洗浄The cake is washed with methanol (6 volumes)
13. 13
    その他dried under vacuum

実験手順

To 1 kg of N-{3-[(2-chloro-5-methoxyphenyl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamide, add a catalytic amount of platinum sulfide on carbon (Pt(S)C), 6 volumes of THF, 0.16 volume of water and 2 volumes of ethanol. The reaction mixture is stirred and heated to reflux. An aqueous potassium formate solution (1.4 volume of water+0.69 kg of potassium formate) is added. The reaction mixture is stirred at reflux until completion of the reaction and cooled down at 50° C. After the addition of 10 volumes of methanol and a one hour stirring, the catalyst is filtered off and washed with 3.4 volumes of methanol. The filtered solution is cooled down at 20° C. 0.62 kg of HCl are added. The reaction mixture is stirred at 20° C., cooled down at 5° C. and filtered. The cake is washed with methanol (6 volumes) and dried under vacuum.

出典