Water → Olanzapine

HRID 1666935Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1666935
[NH2:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[NH:4][C:5]1[S:6][C:7]([CH3:12])=[CH:8][C:9]=1[C:10]#[N:11].ClCCl.O.[CH3:21][N:22]1[CH2:27][CH2:26]N[CH2:24][CH2:23]1>Cl.CN1CCNCC1>[CH3:12][C:7]1[S:6][C:5]2[NH:4][C:3]3[CH:13]=[CH:14][CH:15]=[CH:16][C:2]=3[N:1]=[C:10]([N:11]3[CH2:26][CH2:27][N:22]([CH3:21])[CH2:23][CH2:24]3)[C:9]=2[CH:8]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6344DichloromethaneHCID 531671-MethylpiperazineHCID 674452622-(2-Aminoanilino)-5-methylthiophene-3-carbonitrile

Produkt 1

HCID 135398745Olanzapine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 121968951-Methylpiperazine hydrochlorideLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

2-(2-Aminoanilino)-5-methylthiophene-3-carbonitrile (10.0 g) is taken in N-methyl-piperazine (60 ml) and N-methyl-piperazine hydrochloride (24 gm). The solution is heated at 120° C. until completion of reaction. The reaction mass is cooled and dichloromethane (100 ml) and water is added. The mixture is cooled up to room temperature and dichloromethane layer is separated. 50 ml dichloromethane is evaporated and cyclohexane is added in clear solution. On Cooling the solution, solid is separated out, which is filtered and dried under vacuum to get Olanzapine Form I. (Purity >99.6%)

Aufarbeitung

  1. temperatureThe reaction mass is cooled
  2. temperatureThe mixture is cooled up to room temperature
  3. customdichloromethane layer is separated
  4. custom50 ml dichloromethane is evaporated
  5. additioncyclohexane is added in clear solution
  6. temperatureOn Cooling the solution, solid
  7. customis separated out
  8. filtrationwhich is filtered
  9. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-8deccf48941d4bf2a5acbabb0be7147a
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08044196B2

Notizen zur Reaktion

Wird geladen…