反応 #70198
ord-b4b4c796196d4c9fbabbe5a9f1564cc3
反応方程式
反応条件
後処理
- 1workup.ADDITIONthen treated
- 2温度to warm to 18° C
- 3workup.STIRRINGStirring
- 4洗浄The separated organic phase was washed with H2O (1×10 mL)
- 5乾燥then dried (MgSO4)
- 6ろ過filtered
- 7濃縮concentrated under reduced pressure
実験手順
A mixture of Mg turnings (585 mg, 24.1 g·atom) in dry Et2O (8.0 mL) was stirred at 0° C. under a nitrogen atmosphere then treated, dropwise, with a solution of iodomethane (2.25 mL, 28.1 mmol) in dry Et2O (7.0 mL). After 0.5 h a solution of aldehyde 5 (3.00 g, 9.38 mmol) in dry Et2O (10 mL) was added, dropwise, to the mixture that was then allowed to warm to 18° C. Stirring was continued at this temperature for 3 h then the reaction mixture was treated with NH4Cl (10 mL of a 20% w/v aqueous solution) followed by Et2O (20 mL). The separated organic phase was washed with H2O (1×10 mL) then dried (MgSO4), filtered and concentrated under reduced pressure to afford the title compound 7 (3.19 g, 97%) as an orange oil.