反应详情

To a solution of 5-hydroxy-12H-benzo[a]phenothiazine (2.65 g) and methyl iodide (2.5 ml) in DMF (dimethylformamide) (10 ml) there was added powdered potassium carbonate (2.0 g). The mixture was stirred at room temperature and after 15 minutes, another addition of potassium carbonate (2.0 g) and methyl iodide (2.0 ml) was done. The mixture was stirred for a further 20 minutes, then it was diluted with ethyl acetate (100 ml and washed with water (60 ml) twice, dried and evaporated down. The residue was triturated with ether to afford solid crude product which was filtered (1.7 g). This crude product was chromatographed on a column of silica gel, eluting with dichloromethane to afford pure title compound (1.33 g), m.p. 168°-170° C.

1. stirringThe mixture was stirred for a further 20 minutes
2. washwashed with water (60 ml) twice
3. customdried
4. customevaporated down
5. customThe residue was triturated with ether
6. customto afford solid crude product which
7. filtrationwas filtered (1.7 g)
8. customThis crude product was chromatographed on a column of silica gel
9. washeluting with dichloromethane