تفاعل #949002

معادلة التفاعل

ammonia

water

2-methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride

→

4-Methyl-5-nitrosaccharin

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   أخرىwater and THF are removed by concentration on a rotary evaporator
2. 2
   workup.STIRRINGthe residue which remains is stirred with ethyl acetate
3. 3
   ترشيحfiltered off with suction
4. 4
   غسيلwashed with ethyl acetate
5. 5
   أخرىAfter drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.)
6. 6
   أخرىare obtained

الإجراء التجريبي

104 ml of 25 percent ammonia solution are initially taken, 100 ml of water are added and a solution of 48.7 g (0.166 mol) of 2-methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride in 70 ml of tetrahydrofuran is then added dropwise at 10° C. After stirring at 25° C. for three hours, water and THF are removed by concentration on a rotary evaporator, and the residue which remains is stirred with ethyl acetate, filtered off with suction and washed with ethyl acetate. After drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.) are obtained.

المصدر