反应详情

2-(3-Chlorobenzoylimino)-3-(3-methyl-sulphonylpropyl)-6-trifluoromethoxybenzothiazoline may be prepared in the following way: 75% m-chloro-perbenzoic acid (5.2 g) is added in the course of about 10 minutes, to 2-imino-3-(3-methylthiopropyl)-6-trifluoromethoxybenzothiazoline (3.9 g) in solution in dichloromethane (100 cc) stirred at a temperature close to 20° C. The reaction mixture is brought to the boil for 18 hours. After cooling to a temperature close to 20° C., the precipitate is filtered off and washed with dichloromethane (50 cc) and the filtrate is concentrated to dryness under reduced pressure after washing with 1N sodium hydroxide solution. The oil obtained is crystallised from ethyl acetate. 2-(3-Chlorobenzoylimino)-3-(3-methylsulphonylpropyl)-6-trifluoromethoxybenzothiazoline (0.6 g) melting at 188° C. is obtained.

1. customclose to 20° C
2. temperatureAfter cooling to a temperature
3. customclose to 20° C.
4. filtrationthe precipitate is filtered off
5. washwashed with dichloromethane (50 cc)
6. concentrationthe filtrate is concentrated to dryness under reduced pressure
7. washafter washing with 1N sodium hydroxide solution
8. customThe oil obtained
9. customis crystallised from ethyl acetate