反应详情

温度

0 °C

To 2,4,5-trifluoroaniline (35.0 g) are added anhydrous dichloromethane (530 ml) and dimethyl sulfide (24.6 ml) and the mixture is cooled to 0° C. Thereto N-chlorosuccinimide (38.2 g) is gradually added below 5° C. After the mixture is stirred at the same temperature for 15 minutes, triethylamine (47.7 ml) is gradually added. After reflux for 12 hours, the resultant is made alkaline with 5% aqueous sodium hydroxide solution, extracted with dichloromethane, and the extract is dried over sodium sulfate and concentrated. The residue is purified with column chlomatography (silica-gel, dichloromethane: n-hexane=1: 4) to give 2-methylthiomethyl-3,4,6-trifluoroaniline (22.3 g).

1. customis gradually added below 5° C
2. temperatureAfter reflux for 12 hours
3. extractionextracted with dichloromethane
4. dry with materialthe extract is dried over sodium sulfate
5. concentrationconcentrated
6. customThe residue is purified with column chlomatography (silica-gel, dichloromethane: n-hexane=1: 4)