Reaktion #56062

Reaktionsgleichung

cyclohexanecarboxylic acid

cyclohexanecarbonyl chloride

8-toluyloxy-5-(1-hydroxy-2-isopropylaminobutyl)carbostyril

methanol

→

8-toluyloxy-5-(1-cyclohexylcarbonyloxy-2-isopropylaminobutyl)carbostyril hydrochloride

Lösungsmittel

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto react for 1 hour at a temperature of 80° C
2. 2
   workup.ADDITIONwere added to the reaction mixture
3. 3
   Sonstigeto crystallize the product
4. 4
   SonstigeThe crystals thus obtained
5. 5
   Sonstigewere separated by filtration
6. 6
   Waschenwashed with diethyl ether
7. 7
   Sonstigerecrystallized from a mixture of methanol and diethyl ether

Vorschrift

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.

Quelle