Réaction #56053

ord-56865a89a47345e59c26c3b9497d1994

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas added dropwise to the mixture
  2. 2
    workup.STIRRINGby stirring for 2 hours
  3. 3
    Autrethe precipitate formed
  4. 4
    Lavagewas washed with diethyl ether
  5. 5
    workup.STIRRINGstirred in a small amount of cold water
  6. 6
    AutreThe precipitate was separated by filtration
  7. 7
    Lavagewashed successively with a small amount of water, acetone and diethyl ether
  8. 8
    Autreto obtain a crystalline product which
  9. 9
    Autrewas then recrystallized from acetone

Mode opératoire

50 ml of pyridine was added to 2.5 g of 8-hydroxy-5-(α-isopropylaminobutyryl)carbostyril, and 5 ml of isobutyryl chloride was added dropwise to the mixture while cooling with ice-water and stirring followed by stirring for 2 hours. After addition of about 500 ml of diethyl ether, the precipitate formed was washed with diethyl ether and stirred in a small amount of cold water. The precipitate was separated by filtration, washed successively with a small amount of water, acetone and diethyl ether to obtain a crystalline product which was then recrystallized from acetone to obtain 2.1 g of 8-isobutyryloxy-5-(α-Isopropylaminobutyryl)carbostyril hydrochloride having a melting point of 231°-233° C. (with decomposition).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04223137uspto-grants-1980_09