تفاعل #70218

ord-cfc0d04a7ad44679ae041b23872c8b19

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONthen treated
  2. 2
    درجة الحرارةto warm to 18° C. at which temperature it
  3. 3
    workup.STIRRINGwas stirred for a further 1 h
  4. 4
    غسيلThe separated organic phase was washed with H2O (1×20 mL)
  5. 5
    تجفيفthen dried (MgSO4)
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536157B2uspto-grants-2013_09