反応 #50093

ord-4885e1af76354a0da3de3354ae290034

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONDuring, the addition
  2. 2
    温度for further two hours the temperature of the reaction mixture was maintained at 40° C.
  3. 3
    温度After cooling to room temperature
  4. 4
    抽出the product was extracted into toluene
  5. 5
    洗浄After washing with water until neutral pH
  6. 6
    乾燥drying with anhydrous magnesium sulfate
  7. 7
    その他the solvent was evaporated
  8. 8
    workup.DISTILLATIONthe residue was distilled under diminished pressure

実験手順

To a solution of 362 g of sodium hydroxide in 362 ml of demineralized water 216.6 g of α-isopropyl-2-methylbenzyl cyanide and 6.4 g of tetrabutylammonium hydrogen sulfate were added, and the mixture was heated to 40° C. with intensive stirring. During 3hours 287 g of allylchloride was added. During, the addition and for further two hours the temperature of the reaction mixture was maintained at 40° C. and thereafter at 60° C. for additional three hours. After cooling to room temperature, the reaction mixture was diluted with 550 ml of water and the product was extracted into toluene. After washing with water until neutral pH and drying with anhydrous magnesium sulfate, the solvent was evaporated and the residue was distilled under diminished pressure to obtain 249 g (93%) of the desired compound, b.p. 122°-124 ° C./333 Pa.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05424456uspto-grants-1995_06