반응 #452449

ord-36f903ae0afc4ed6b419143fa000bc71

반응 조건

온도
30°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A 250-ml round-bottomed flask fitted with a condenser
  2. 2
    기타The resulting reaction mixture
  3. 3
    기타after which time the solvent was removed under reduced pressure
  4. 4
    온도The residue, a white solid, was maintained at 0.01 Torr for 30 minutes
  5. 5
    기타to remove residual solvent and excess thionyl chloride

실험 절차

A 250-ml round-bottomed flask fitted with a condenser was charged with 12.0 g of 1-hydroxycyclohexyl 4-(2-carboxyethyl)carbonylphenyl ketone (0.04 mole), 5.95 g (0.05 mole) of thionyl chloride (Aldrich Chemical Co., Milwaukee, Wis.), and 50 ml of diethyl ether. The resulting reaction mixture was stirred at 30° C. for 30 minutes, after which time the solvent was removed under reduced pressure. The residue, a white solid, was maintained at 0.01 Torr for 30 minutes to remove residual solvent and excess thionyl chloride, leaving 12.1 g (94 percent) of 1-hydroxycyclohexyl 4-(2-chloroformylethyl)carbonylphenyl ketone.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06127073uspto-grants-2000_10