تفاعل #5616

ord-2ef62d98fe1447439390fdc1af915ab7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITThe stirring was continued for an hour at -18°~12° C
  2. 2
    أخرىThe resulting precipitates
  3. 3
    ترشيحwere collected by filtration
  4. 4
    غسيلwashed with diisopropyl ether
  5. 5
    تجفيفdried over phosphorus pentoxide

الإجراء التجريبي

To a suspension of phosphorus pentachloride (4.6 g) in methylene chloride (40 ml) was added 4,5-diacetoxy-2-pyridinecarboxylic acid (4.5 g) at -20° C. with stirring. The stirring was continued for an hour at -18°~12° C. To the reaction mixture was added diisopropyl ether (80 ml) below 0° C. The resulting precipitates were collected by filtration, washed with diisopropyl ether and dried over phosphorus pentoxide to give 4,5-diacetoxy-2-pyridinecarbonyl chloride hydrochloride (5.15 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05244890uspto-grants-1993_09