反应详情

温度

27.5 °C

3-Chloro-1-(4-octylphenyl)propan-1-one obtained in Example 1 and dimethylformamide (250 mL) are charged into a round bottom flask and stirred for dissolution at 25-30° C. Sodium nitrite (25.66 g) is charged into the flask and the reaction mixture is stirred 25-30° C. for about 90 minutes. The reaction mixture is added to a mixture of water (500 mL) precooled to 0-5° C. and ethyl acetate (250 mL), stirred, and the organic layer is separated. The aqueous layer is extracted with ethyl acetate (250 mL) and the organic layer is combined with the initial organic layer. The combined organic layer is washed with water (250 mL) followed by brine solution (100 mL), dried over sodium sulphate (50 g), and evaporated under reduced pressure at 45° C. to obtain the crude compound. The crude compound is dissolved in hexane (500 mL) at 26° C., is cooled to −10° C., and stirred for about 40 minutes at the same temperature. The obtained solid is filtered, washed with precooled hexane (100 mL), and dried at 26° C. to give 37.0 g of the title compound.

1. stirringthe reaction mixture is stirred 25-30° C. for about 90 minutes
2. customprecooled to 0-5° C.
3. customthe organic layer is separated
4. extractionThe aqueous layer is extracted with ethyl acetate (250 mL)
5. washThe combined organic layer is washed with water (250 mL)
6. dry with materialdried over sodium sulphate (50 g)
7. customevaporated under reduced pressure at 45° C.
8. customto obtain the crude compound
9. temperatureis cooled to −10° C.
10. stirringstirred for about 40 minutes at the same temperature
11. filtrationThe obtained solid is filtered
12. washwashed with precooled hexane (100 mL)
13. customdried at 26° C.