反应详情

A suspension of 21.75 g (83.9 mmol) of 3,7-dimethoxyphenothiazine, 43.36 g (0.34 mmol) of dried, powdered potassium carbonate, 25.22 g (0.20 mol) of dimethyl sulphate and 1.35 g (4.19 mmol) of tris-[2-(2-methoxyethoxy)ethyl]amine in 300 ml of toluene was stirred at 110° for 1 hour, then cooled and poured into 1 l of ice-water. The mixture was acidified slightly with 2N hydrochloric acid solution and extracted with ethyl acetate. The combined organic phases were extracted with saturated sodium chloride solution, dried over magnesium sulphate and evaporated. The residue was crystallized from ethanol/acetone, whereupon, after drying, 18.4 g (80.2%) of 3,7-dimethoxy-10-methylphenothiazine were obtained as a white solid of m.p. 166°-167°.

1. customof dried
2. temperaturecooled
3. extractionextracted with ethyl acetate
4. extractionThe combined organic phases were extracted with saturated sodium chloride solution
5. dry with materialdried over magnesium sulphate
6. customevaporated
7. customThe residue was crystallized from ethanol/acetone, whereupon
8. customafter drying