反応 #904

反応方程式

ammonia

water

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

→

4-Methyl-5-nitrosaccharin

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   濃縮the mixture is concentrated on a rotary evaporator
2. 2
   その他to remove water and THF
3. 3
   workup.STIRRINGThe residue which remains is stirred with ethyl acetate
4. 4
   ろ過filtered off with suction
5. 5
   洗浄washed with ethyl acetate
6. 6
   その他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
   その他are obtained

実験手順

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.

出典