反应详情

4,4,5-trimethyl-cyclohexane-1,3-dione (0.98 g, 6.36 mmole) and triethylamine (0.77 g, 7.26 mmole) were dissolved in methylene chloride (30 ml). Into the resulting solution cooled with ice, a methylene chloride solution (5 ml) of 2-nitro-4-methylsulfonylbenzoyl chloride (1.68 g, 6.38 mmole) was dropped, and then this solution was stirred at room temperature for an hour. The resulting solution was washed with water, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in acetonitrile (40 ml), into which triethylamine (0.77 g, 7.62 mmole) and potassium cyanide (0.1 g, 1.54 mmole) were added to stir at room temperature for 16 hours. The reaction solution was concentrated under reduced pressure. The residue was dissolved by adding ethyl acetate and water. To the resulting solution, diluted hydrochloric acid was added until the aqueous layer became acidic (pH 2 or below). The organic layer was washed with water, dried with anhydrous magnesium sulfate and concentrated under reduced pressure. Methanol was added to the residue to crystallize to give crystal (0.57 g, mp: 166°-7° C.).

1. temperatureInto the resulting solution cooled with ice
2. washThe resulting solution was washed with water
3. dry with materialdried with anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. additionwere added
6. stirringto stir at room temperature for 16 hours
7. concentrationThe reaction solution was concentrated under reduced pressure
8. dissolutionThe residue was dissolved
9. additionby adding ethyl acetate and water
10. additionTo the resulting solution, diluted hydrochloric acid was added until the aqueous layer
11. washThe organic layer was washed with water
12. dry with materialdried with anhydrous magnesium sulfate
13. concentrationconcentrated under reduced pressure
14. additionMethanol was added to the residue
15. customto crystallize