Water → 4-amino-5-chloro-N-[(3R,4S)-1-[3-(4-fluorophenoxy)propyl]-3-methoxypiperidin-4-yl]-2-methoxybenzamide

HRID 1088410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1088410
O.[NH2:2][C:3]1[C:30]([Cl:31])=[CH:29][C:6]([C:7]([NH:9][C@H:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=3)[CH2:12][C@H:11]2[O:27][CH3:28])=[O:8])=[C:5]([O:32][CH3:33])[CH:4]=1.O>CC1C=CC=CC=1>[NH2:2][C:3]1[C:30]([Cl:31])=[CH:29][C:6]([C:7]([NH:9][C@H:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:21]=[CH:22][C:23]([F:26])=[CH:24][CH:25]=3)[CH2:12][C@H:11]2[O:27][CH3:28])=[O:8])=[C:5]([O:32][CH3:33])[CH:4]=1

Komponenten

4

Edukt 2

HCID 962WaterHCID 13677778Alimix

Produkt 1

HCID 53110474-amino-5-chloro-N-[(3R,4S)-1-[3-(4-fluorophenoxy)propyl]-3-methoxypiperidin-4-yl]-2-methoxybenzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

30 Parts of cis-4-amino-5-chloro-N-[1-[3-(4-fluorophenoxy)propyl]-3-methoxy-4-piperidinyl]-2-methoxybenzamide monohydrate were dissolved in 280 parts of methylbenzene at reflux temperature and the solution was stirred and refluxed for 2 hours using a water-separator. 180 Parts of methylbenzene were distilled off. The residue was allowed to cool overnight while stirring. The solid product was filtered off and boiled for 1.50 hours in heptane. The product was filtered off and dried, yielding 23.1 parts of cis-4-amino-5-chloro-N-[1-[3-(4-fluorophenoxy)propyl]-3-methoxy-4-piperidinyl]-2-methoxybenzamide; mp. 131.7°-33° C. (compound 245).

Aufarbeitung

  1. temperatureat reflux temperature
  2. temperaturerefluxed for 2 hours
  3. distillation180 Parts of methylbenzene were distilled off
  4. temperatureto cool overnight
  5. stirringwhile stirring
  6. filtrationThe solid product was filtered off
  7. filtrationThe product was filtered off
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3d4b251978f645fd93ef905daf576ff5
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04962115

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