تفاعل #350546

ord-3e05d738ccd7441ba447fdb10098ccb2

المذيبات

ظروف التفاعل

درجة الحرارة
30°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05643356uspto-grants-1997_07