반응 #683589

ord-c11f6eaa7d8b461bbcde09014bde7bcb

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타In a one liter three-neck flask provided with agitating means
  2. 2
    workup.ADDITIONwere charged
  3. 3
    workup.ADDITIONwas added dropwise to the flask
  4. 4
    기타kept at 160° C
  5. 5
    workup.ADDITIONafter the completion of the addition at the same temperature
  6. 6
    세척washed with water
  7. 7
    workup.ADDITIONafter the addition of 500 ml of petroleum ether and 500 ml of water
  8. 8
    workup.STIRRINGwith stirring
  9. 9
    기타The petroleum ether layer was separated
  10. 10
    workup.DISTILLATIONwhich was distilled under a reduced pressure
  11. 11
    건조after being dried with anhydrous sodium sulfate

실험 절차

In a one liter three-neck flask provided with agitating means were charged and stirred 216 g (1.5 mole) of α-naphthol and 171 g (1.26 mole) of zinc chloride, 278 g (1.26 mole) of tetradecyl alcohol was added dropwise to the flask kept at 160° C. Stirring was continued for 8 hours after the completion of the addition at the same temperature. The reaction product was cooled to room temperature (i.e., 20°-30° C), and then washed with water after the addition of 500 ml of petroleum ether and 500 ml of water with stirring. This washing operation was repeated twice. The petroleum ether layer was separated, which was distilled under a reduced pressure after being dried with anhydrous sodium sulfate. 183 g of 4-tetradecyl-α-naphthol (yield: 42.7%) having boiling range of 188° to 194° C at 0.15 mmHg was obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04011082uspto-grants-1977_03