تفاعل #56062

ord-e216a3fa8265425bb0145043269e4986

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.ADDITIONwere 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 methanol and diethyl ether

الإجراء التجريبي

2 ml of cyclohexanecarboxylic acid and 2 ml of cyclohexanecarbonyl chloride were added to 1 g of 8-toluyloxy-5-(1-hydroxy-2-isopropylaminobutyl)carbostyril and the mixture was allowed to react for 1 hour at a temperature of 80° C. After completion of the reaction, 2 to 3 drops of concentrated hydrochloric acid and 10 ml of methanol were 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 methanol and diethyl ether to obtain 1.3 g of 8-toluyloxy-5-(1-cyclohexylcarbonyloxy-2-isopropylaminobutyl)carbostyril hydrochloride having a melting point of 231°-232.5° C.

المصدر

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