Water → Olanzapine

HRID 1666934Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1666934
[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].O1[CH2:21][CH2:20]CC1.O>CN1CCNCC1.C(O)(=O)C>[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[CH2:21][CH2:20][N:4]([CH3:5])[CH2:3][CH2:2]3)[C:9]=2[CH:8]=1

Komponenten

6

Edukt 3

HCID 962WaterHCID 8028TetrahydrofuranHCID 674452622-(2-Aminoanilino)-5-methylthiophene-3-carbonitrile

Produkt 1

HCID 135398745Olanzapine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 531671-MethylpiperazineLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

2-(2-Aminoanilino)-5-methylthiophene-3-carbonitrile (2.0 g) is taken in N-methyl-piperazine (12 ml) and acetic acid (2 ml). The solution is heated at 120° C. until completion of reaction. The reaction mass is cooled and tetrahydrofuran is added. The reaction mixture is stirred for 30 minutes. The water is added at 45-50° C., the mixture is cooled up to room temperature and the solid is precipitated out. The solid is filtered off and washed with tetrahydrofuran-water mixture.

Aufarbeitung

  1. temperatureThe reaction mass is cooled
  2. temperaturethe mixture is cooled up to room temperature
  3. customthe solid is precipitated out
  4. filtrationThe solid is filtered off
  5. washwashed with tetrahydrofuran-water mixture

Quellen und Nachweise

ORD-Eintrag
ord-4f6f788d2859416faafff9e38b301e71
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08044196B2

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