反应详情

A solution of 12.6 g of 2,2-dimethyl-4-(1,2,4-triazol-1-yl)-8-phenoxyoctan-3-one was added dropwise to a solution of 8.7 g of vinyl magnesium chloride in 70 ml of tetrahydrofuran, while stirring. After the weakly exothermic reaction was complete, the mixture was refluxed for a further 5 hours and then cooled. Thereafter, a mixture of 5 ml of water and 5 ml of tetrahydrofuran was added dropwise, while cooling with ice, the reaction mixture was stirred for a further 2 hours at room temperature, the precipitated magnesium salts were then filtered off, and the filtrate was concentrated under reduced pressure. The residue from the filtrate was taken up in 100 ml of dichloromethane, the solution was washed with 100 ml of water and then with 100 ml of saturated ammonium chloride solution, and the organic phase was dried over magnesium sulfate and then concentrated under reduced pressure. 8.0 g of pale yellowish crystals of melting point 66°-69° C. (diastereomer mixture 2:1) crystallized from the residual oil on trituration with diisopropyl ether.

1. customAfter the weakly exothermic reaction
2. temperaturethe mixture was refluxed for a further 5 hours
3. temperaturecooled
4. additionwas added dropwise
5. temperaturewhile cooling with ice
6. stirringthe reaction mixture was stirred for a further 2 hours at room temperature
7. filtrationthe precipitated magnesium salts were then filtered off
8. concentrationthe filtrate was concentrated under reduced pressure
9. washthe solution was washed with 100 ml of water
10. dry with materialwith 100 ml of saturated ammonium chloride solution, and the organic phase was dried over magnesium sulfate
11. concentrationconcentrated under reduced pressure
12. custom8.0 g of pale yellowish crystals of melting point 66°-69° C. (diastereomer mixture 2:1) crystallized from the residual oil on trituration with diisopropyl ether