반응 #70218

ord-cfc0d04a7ad44679ae041b23872c8b19

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONthen treated
  2. 2
    온도to warm to 18° C. at which temperature it
  3. 3
    workup.STIRRINGwas stirred for a further 1 h
  4. 4
    세척The separated organic phase was washed with H2O (1×20 mL)
  5. 5
    건조then dried (MgSO4)
  6. 6
    여과filtered
  7. 7
    농축concentrated under reduced pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536157B2uspto-grants-2013_09