反应详情

A solution of 3,6-dichloro-4H-thieno[3,2-e]-1,2,4-thiadiazine 1,1-dioxide (0.5 g, 1.94 mmol) in 1,2-dimethylpropylamine (5 ml) was stirred for 48 h at 100° C in a sealed flask. The cooled mixture was concentrated in vacuo and the residue was stirred with water (20 ml) followed by adjustment to pH 2 with 4M hydrochloric acid. The initially formed gummy product crystallised by stirring the mixture for about 2 h at 0° C. The precipitate was isolated by filtration, washed with water, and recrystallised from ethyl acetate/methanol followed by drying in vacuo at 60° C. over night to give 0.43 g (72%) of the pure title compound.

1. concentrationThe cooled mixture was concentrated in vacuo
2. customThe initially formed gummy product crystallised
3. stirringby stirring the mixture for about 2 h at 0° C
4. customThe precipitate was isolated by filtration
5. washwashed with water
6. customrecrystallised from ethyl acetate/methanol
7. customby drying in vacuo at 60° C. over night