Potassium Carbonate → 3-(4-chloro-7H-pyrrolo[2,3-d]pyrimidin-5-yl)benzonitrile

HRID 1750273

Reaktionsgleichung

Reaktionsgleichung von HRID 1750273
[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]=1

Komponenten

4

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

  1. customSolvent was removed in vacuo
  2. additionthe residue was mixed with water (100 mL)
  3. customThe resulting solid was isolated via filtration
  4. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-bcebf8b53d9c434fa914b4837a4768b4
Quelldatensatz
uspto-grants-2015_10
Patentnummer
US09156845B2

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