反応 #89602

ord-8c68af2af581457a9ac1b265fab608e2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was then fed for over 2 hours at 0° C. under nitrogen
  2. 2
    その他quenched
  3. 3
    workup.ADDITIONby pouring the reaction mixture onto a sulfuric acid solution (10%)
  4. 4
    その他on crushed ice
  5. 5
    その他The organic layer was separated
  6. 6
    洗浄washed with sodium carbonate solution
  7. 7
    workup.DISTILLATIONdistilled

実験手順

Isopropylmagnesium chloride ((CH3)2HCMgCl) in tetrahydrofuran (THF) (1.6 L, 3.2 mol) was loaded into a flame-dried 5 L round bottom flask. Additional THF (1 L) was added. 1-Isopropyl-2,4-dimethyl-cyclohex-3-enecarbaldehyde (obtained as detailed above) was then fed for over 2 hours at 0° C. under nitrogen. The reaction mixture was aged at 0° C. for another 3 hours and then quenched by pouring the reaction mixture onto a sulfuric acid solution (10%) on crushed ice. The organic layer was separated, washed with sodium carbonate solution, and distilled to provide (1-isopropyl-2,4-dimethyl-cyclohex-3-enyl)-methanol.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09441185B2uspto-grants-2016_09