反应 #904

反应方程式

ammonia

water

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

→

4-Methyl-5-nitrosaccharin

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   浓缩the mixture is concentrated on a rotary evaporator
2. 2
   其他to remove water and THF
3. 3
   workup.STIRRINGThe residue which remains is stirred with ethyl acetate
4. 4
   过滤filtered off with suction
5. 5
   洗涤washed with ethyl acetate
6. 6
   其他After drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.)
7. 7
   其他are obtained

实验过程

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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