تفاعل #904

معادلة التفاعل

ammonia

water

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

→

4-Methyl-5-nitrosaccharin

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   تركيزthe mixture is concentrated on a rotary evaporator
2. 2
   أخرىto remove water and THF
3. 3
   workup.STIRRINGThe residue which remains is stirred with ethyl acetate
4. 4
   ترشيحfiltered off with suction
5. 5
   غسيلwashed with ethyl acetate
6. 6
   أخرىAfter drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.)
7. 7
   أخرىare obtained

الإجراء التجريبي

104 ml of 25% 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, the mixture is concentrated on a rotary evaporator to remove water and THF. 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