تفاعل #56063

ord-8294f87b96c34758a9476c5d5ebb2992

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto react for 1 hour at a temperature of 80° C
  2. 2
    workup.ADDITIONwas added to the reaction mixture
  3. 3
    أخرىto crystallize the product
  4. 4
    أخرىThe crystals thus obtained
  5. 5
    أخرىwere separated by filtration
  6. 6
    غسيلwashed with diethyl ether
  7. 7
    أخرىrecrystallized from a mixture of ethanol and acetone

الإجراء التجريبي

2 ml of cyclopropanecarboxylic acid and 1 ml of cyclopropanecarboxylic acid chloride were added to 500 mg of 5-[1-hydroxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-hydroxycarbostyril hydrochloride, and the mixture was allowed to react for 1 hour at a temperature of 80° C. After completion of the reaction, 10 ml of methanol was added to the reaction mixture while cooling with ice-water followed by addition of diethyl ether to crystallize the product. The crystals thus obtained were separated by filtration, washed with diethyl ether and recrystallized from a mixture of ethanol and acetone to obtain 210 mg of 5-[1-cyclopropylcarbonyloxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-cyclopropylcarbonyloxycarbostyril hydrochloride having a melting point of 167°-168° C. (with decomposition).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04223137uspto-grants-1980_09