反应详情

温度

0 °C

0.76 g of 2,2-difluoro-6-[(4,5-dimethoxy-2-pyridyl)methylthio]-5H-[1,3]-dioxolo[4,5-f]benzimidazole are dissolved in 10 ml of dioxane and 2 ml of 1N sodium hydroxide solution. An equimolar amount of a titrated aqueous sodium hypochlorite solution, to which 1 mole per liter of sodium hydroxide solution has been added, is first added dropwise, while cooling with ice, and after one hour a further equivalent and after 3 hours half the equimolar amount of sodium hypochlorite are added, to achieve complete reaction. After a reaction time of 4 hours, 5 ml of 5% strength sodium thiosulfate solution and another 25 ml of dioxane are added and the upper dioxane phase is separated off, washed once with 5 ml of sodium thiosulfate solution and concentrated on a rotary evaporator. The oily residue is dissolved in 20 ml of water and 10 ml of ethyl acetate and the solution is brought to pH 7 with about 100 ml of a buffer solution of pH 6.8. The solid which has precipitated out is filtered off with suction over a suction filter, washed with water, extracted by stirring at 0° C. with acetone and dried. 0.7 g (87% of theory) of the title compound is obtained in the form of colorless crystals; decomp. at 211°-213° C.

1. additionis first added dropwise
2. temperaturewhile cooling with ice
3. customreaction
4. customthe upper dioxane phase is separated off
5. washwashed once with 5 ml of sodium thiosulfate solution
6. concentrationconcentrated on a rotary evaporator
7. dissolutionThe oily residue is dissolved in 20 ml of water
8. customThe solid which has precipitated out
9. filtrationis filtered off with suction over a suction
10. filtrationfilter
11. washwashed with water
12. extractionextracted
13. customdried