Potassium Iodide → Risperidone

HRID 840434

Reaktionsgleichung

Reaktionsgleichung von HRID 840434
[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]3)=[N:7][O:8][C:4]=2[CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+].[CH3:25][N:26]([CH:28]=[O:29])[CH3:27]>O>[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:10][CH2:11][N:12]([CH2:3][CH2:4][C:5]4[C:28](=[O:29])[N:26]5[CH2:27][CH2:15][CH2:16][CH2:2][C:25]5=[N:7][C:6]=4[CH3:9])[CH2:13][CH2:14]3)=[N:7][O:8][C:4]=2[CH:3]=1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 8494213-(4-Piperidyl)-6-fluoro-1,2-benzisoxazole

Produkt 1

HCID 5073RisperidoneAusbeute 46 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 5.3 parts of 3-(2-chloromethyl)-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one monohydrochloride, 4.4 parts of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole, 8 parts of sodium carbonate, 0.1 part of potassium iodide, and 90 parts of DMF is stirred overnight at 80°-90° C. After cooling, the reaction mixture is poured into water. The product is filtered off and crystallized from a mixture of DMF and 2-propanol. The product is filtered off and dried, yielding 3.8 parts (46%) of 3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one; mp. 170.0° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationThe product is filtered off
  3. customcrystallized from a mixture of DMF and 2-propanol
  4. filtrationThe product is filtered off
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-eb8a8d007ade4cd8b343f5c01bec9ca5
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06368632B1

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