反应详情

The mixture (6.48 g) containing 1,3-benzodioxol-5,6-diamine obtained in the step (78b) above was dissolved in methanol (100 ml). To the mixture, carbon disulfide (30 ml) was added and the mixture was stirred at room temperature for one day. The reaction mixture was concentrated under reduced pressure. To the solid residue, ethyl acetate was added and filtration was performed. The solid was washed by adding tetrahydrofuran, ethyl acetate and diluted hydrochloric acid and insoluble substance was collected by filtration, dried under reduced pressure at room temperature for 2 hours in a desiccator to obtain the title compound (3.8 g, 56.1% from 5,6-dinitro-1,3-benzodioxol) as a brown solid.

1. customobtained in the step (78b)
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionTo the solid residue, ethyl acetate was added
4. filtrationfiltration
5. washThe solid was washed
6. additionby adding tetrahydrofuran, ethyl acetate and diluted hydrochloric acid and insoluble substance
7. filtrationwas collected by filtration
8. customdried under reduced pressure at room temperature for 2 hours in a desiccator