반응 #219171
ord-bc1689beeb9d4730bb23488d2b6ff9ca
반응 방정식
piperidine hydrochloride
4-methylpropiophenone
1,3-dioxolane
hydrochloric acid
→
Tolperisone Hydrochloride
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONa suspension of the product
- 2기타is produced
- 3기타After that the solid is separated from the liquid as a damp product
- 4건조dried 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
- 5기타are isolated
실험 절차
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.