반응 #904

반응 방정식

ammonia

water

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

→

4-Methyl-5-nitrosaccharin

용매

tetrahydrofuran

반응 조건

후처리

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

실험 절차

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.

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