반응 #50093

ord-4885e1af76354a0da3de3354ae290034

반응 방정식

[Na+].[OH-]
sodium hydroxide
Cc1ccccc1C(C#N)C(C)C
α-isopropyl-2-methylbenzyl cyanide
C=CCCl
allylchloride
C=CCC(C#N)(c1ccccc1C)C(C)C
desired compound
수율 93.0%
C=CCC(C#N)(c1ccccc1C)C(C)C
α-Allyl-α-isopropyl-2-methylbenzyl cyanide
수율 93.0%

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONDuring, the addition
  2. 2
    온도for further two hours the temperature of the reaction mixture was maintained at 40° C.
  3. 3
    온도After cooling to room temperature
  4. 4
    추출the product was extracted into toluene
  5. 5
    세척After washing with water until neutral pH
  6. 6
    건조drying with anhydrous magnesium sulfate
  7. 7
    기타the solvent was evaporated
  8. 8
    workup.DISTILLATIONthe residue was distilled under diminished pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05424456uspto-grants-1995_06