반응 #64042

ord-f1f47e8355734a17843cc0977077ff83

반응 조건

온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the aqueous phase was extracted with chloroform (50 ml)
  2. 2
    건조The organic phase was dried over anhydrous sodium sulphate
  3. 3
    기타the solvent was removed by evaporation under reduced pressure
  4. 4
    기타a rotary evaporator

실험 절차

A solution of 3-hydroxy-5-mesityl-2-propionylcyclohex-2-en-1-one (1.8 g) in chloroform (20 ml) was stirred and cooled to 0° C. during the dropwise addition of chlorosulphonic acid (10 ml). The mixture was stirred for four hours at 20° C. and then poured into ice-water and the aqueous phase was extracted with chloroform (50 ml). The organic phase was dried over anhydrous sodium sulphate and the solvent was removed by evaporation under reduced pressure using a rotary evaporator. The product 3-hydroxy-5-(2,4,6-trimethyl-3-chlorosulphonylphenyl)-2-propionylcyclohex-2-en-1-one was isolated as a brown oil (2.4 g, 97%). Proton magnetic resonance spectrum (CDCl3 ; δ in ppm): 1.16 (3H, t); 2.47 (3H, s); 2.69 (3H, s); 2.80 (3H, s); 2.7-4.0 (7H, m); 7.05 (1H, s); 18.30 (1H, s).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04767879uspto-grants-1988_08