반응 #742283

ord-0ac3c5a76c6847c08842e52140f5c964

반응 방정식

O=P(O)(O)O
Phosphoric acid
C=CC1(C)CC=C(C)CC1
1,4-dimethyl-4-vinyl-cyclohexene
CC1=CCC2(C)CCC1C2
2,5-dimethyl-bicyclo[3.2.1]oct-2-ene

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was subsequently quenched with a solution of sodium hydroxide (NaOH)
  2. 2
    기타The organic layer was separated
  3. 3
    건조dried over sodium sulfate (Na2SO4)

실험 절차

Phosphoric acid (H3PO4, 145 g, 1.48 mol) was added to a solution of 1,4-dimethyl-4-vinyl-cyclohexene (403 g, 2.96 mol, commercially available from Evonik Industries) in toluene (500 mL) and refluxed for 6 hours. The reaction mixture was subsequently quenched with a solution of sodium hydroxide (NaOH). The organic layer was separated, dried over sodium sulfate (Na2SO4), and fractionated to provide 2,5-dimethyl-bicyclo[3.2.1]oct-2-ene (280 g) having a boiling point of 87° C. at a pressure of 27 mmHg

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08071529B1uspto-grants-2011_12