Reaktionsgleichung
[Cl:1][C:2]1[C:3]2[C:10]([C:11]3[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=3)[C:14]#[N:15])=[CH:9][N:8](CO)[C:4]=2[N:5]=[CH:6][N:7]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:1][C:2]1[C:3]2[C:10]([C:11]3[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=3)[C:14]#[N:15])=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 3-[4-chloro-7-(hydroxymethyl)-7H-pyrrolo[2,3-d]pyrimidin-5-yl]benzonitrile (C13) (4 g from the previous step, ≦9.9 mmol) in methanol (100 mL) was adjusted to pH>12 by addition of solid potassium carbonate. Solvent was removed in vacuo and the residue was mixed with water (100 mL). The resulting solid was isolated via filtration and washed with water, providing the product as a white solid. Yield: 1.3 g, 5.1 mmol, 52% over two steps. LCMS m/z 255.0 [M+H+].
Aufarbeitung
- customSolvent was removed in vacuo
- additionthe residue was mixed with water (100 mL)
- customThe resulting solid was isolated via filtration
- washwashed with water
Quellen und Nachweise
- ORD-Eintrag
- ord-bcebf8b53d9c434fa914b4837a4768b4
- Quelldatensatz
- uspto-grants-2015_10
- Patentnummer
- US09156845B2
Verknüpfte Notizen
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