반응 #1092

반응 방정식

potassium hydroxide

2-methoxycarbonyl-5-nitrobenzenesulfonic acid

phosphorus oxychloride

→

2-Methoxycarbonyl-5-nitrobenzenesulfonyl chloride

용매

methanol

methanol

반응 조건

후처리

1. 1
   기타the salt which is precipitated
2. 2
   여과is filtered off
3. 3
   기타dried
4. 4
   온도the mixture is heated
5. 5
   기타The 2-methoxycarbonyl-5-nitrobenzenesulfonyl chloride (60.1 g, 70% of theory) which has precipitated
6. 6
   여과is filtered off with suction through a Buchner funnel

실험 절차

A solution of 17.3 g (0.27 mol) of potassium hydroxide (88% strength) and 100 ml of methanol is added carefully with vigorous stirring to a solution of 70.9 g (0.27 mol) of 2-methoxycarbonyl-5-nitrobenzenesulfonic acid in 300 ml of methanol. The mixture is cooled to 0° C. and the salt which is precipitated is filtered off, dried and then suspended in 150 ml of sulfolane, 150 ml of acetonitrile and 10 ml of dimethylformamide. After the dropwise addition of 100 ml (1.07 mol) of phosphorus oxychloride, the mixture is heated at boiling for 2.5 h. The reaction mixture is then poured into ice-water. The 2-methoxycarbonyl-5-nitrobenzenesulfonyl chloride (60.1 g, 70% of theory) which has precipitated is filtered off with suction through a Buchner funnel and freed from traces of solvent under reduced pressure. Melting point: 86°-88° C.

출처