Реакция #64042

ord-f1f47e8355734a17843cc0977077ff83

Растворители

Условия реакции

Температура
20°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияthe aqueous phase was extracted with chloroform (50 ml)
  2. 2
    СушкаThe organic phase was dried over anhydrous sodium sulphate
  3. 3
    Другоеthe solvent was removed by evaporation under reduced pressure
  4. 4
    Другоеa rotary evaporator

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04767879uspto-grants-1988_08