تفاعل #70218
ord-cfc0d04a7ad44679ae041b23872c8b19
معادلة التفاعل
الكواشف
ظروف التفاعل
المعالجة
- 1workup.ADDITIONthen treated
- 2درجة الحرارةto warm to 18° C. at which temperature it
- 3workup.STIRRINGwas stirred for a further 1 h
- 4غسيلThe separated organic phase was washed with H2O (1×20 mL)
- 5تجفيفthen dried (MgSO4)
- 6ترشيحfiltered
- 7تركيزconcentrated under reduced pressure
الإجراء التجريبي
A mixture of Mg turnings (231 mg, 9.51 g·atom) in dry Et2O (3.0 mL) was stirred at 0° C. under a nitrogen atmosphere then treated, dropwise, with a solution of iodomethane (680 μL, 10.9 mmol) in dry Et2O (2.0 mL). After 0.5 h a solution of aldehyde 36 (1.00 g, 3.66 mmol) in dry Et2O (10 mL) was added, dropwise, to the reaction mixture that was then allowed to warm to 18° C. at which temperature it was stirred for a further 1 h. After this time NH4Cl (15 mL of a 20% w/v aqueous solution) then Et2O (20 mL) were added to the reaction mixture. The separated organic phase was washed with H2O (1×20 mL) then dried (MgSO4), filtered and concentrated under reduced pressure to afford the title compound 37 (1.05 g, 99%) as an orange oil.