Hydrochloric Acid → Tolperisone Hydrochloride

HRID 131989

반응식

HRID 131989 반응식
[ClH:1].[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[CH3:8][CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1)=[O:11].O1CCO[CH2:20]1.Cl>CC(OC)(C)C.C(OCC)(=O)C>[CH3:18][C:15]1[CH:16]=[CH:17][C:12]([C:10]([CH:9]([CH2:20][N:2]2[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]2)[CH3:8])=[O:11])=[CH:13][CH:14]=1.[ClH:1]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 125861,3-DioxolaneHCID 21429p-MethylpropiophenoneHCID 2723721Piperidine, hydrochloride (1:1)

생성물 1

HCID 92965Tolperisone Hydrochloride

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 15413tert-Butyl methyl ether용매

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.

후처리

  1. additiona suspension of the product
  2. customis produced
  3. customAfter that the solid is separated from the liquid as a damp product
  4. dry with materialdried 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. customare isolated

출처 및 근거

ORD 기록
ord-bc1689beeb9d4730bb23488d2b6ff9ca
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07385060B2

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