Réaction #219171

ord-bc1689beeb9d4730bb23488d2b6ff9ca

Équation de réaction

C1CCNCC1.Cl
piperidine hydrochloride
CCC(=O)c1ccc(C)cc1
4-methylpropiophenone
C1COCO1
1,3-dioxolane
Cl
hydrochloric acid
Cc1ccc(C(=O)C(C)CN2CCCCC2)cc1.Cl
Tolperisone Hydrochloride

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONa suspension of the product
  2. 2
    Autreis produced
  3. 3
    AutreAfter that the solid is separated from the liquid as a damp product
  4. 4
    Séchagedried at 60-80° C. in the vacuum oven (200-500 mbar) over a period of 12-24 hours whereby 140 kg (81.5%) of colorless crystals
  5. 5
    Autreare isolated

Mode opératoire

75 kg piperidine hydrochloride and 105 kg 4-methylpropiophenone are heated to 90° C. with 180 kg of 1,3-dioxolane and 12 kg of hydrochloric acid under a nitrogen atmosphere for 7 to 20 hours. With addition of 500 kg of ethyl acetate and 440 kg MTBE at a temperature in the range of (40-80° C.), a suspension of the product is produced. After that the solid is separated from the liquid as a damp product and then dried at 60-80° C. in the vacuum oven (200-500 mbar) over a period of 12-24 hours whereby 140 kg (81.5%) of colorless crystals are isolated.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07385060B2uspto-grants-2008_06