Reaktion #88366

Reaktionsgleichung

propane-1-sulfonic acid {2,4-difluoro-3-[5-(1H-indazol-5-yl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl]-phenyl}-amide

acetic anhydride

→

desired compound

propane-1-sulfonic acid {3-[5-(1-acetyl-1H-indazol-5-yl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl]-2,4-difluoro-phenyl}-amide

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated under vacuum
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   TrocknenThe organic layer is dried over sodium sulfate
4. 4
   Filtrationfiltered
5. 5
   Einengenthe filtrate concentrated under vacuum
6. 6
   SonstigeThe resulting material is purified by silica gel column chromatography
7. 7
   Wascheneluting with a gradient of 20-100% ethyl acetate (with 2% acetic acid) in hexanes
8. 8
   Einengenconcentrated under vacuum
9. 9
   Waschenthe resulting solid is further washed with a mixture of ethyl acetate

Vorschrift

Into a round bottom flask, propane-1-sulfonic acid {2,4-difluoro-3-[5-(1H-indazol-5-yl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl]-phenyl}-amide (P-0001, 0.020 g, 0.040 mmol) is combined with acetic anhydride (0.023 mL, 0.24 mmol) and 4 mL of acetonitrile. The reaction is stirred at room temperature for 3 hours, then concentrated under vacuum, combined with water and extracted with ethyl acetate. The organic layer is dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with a gradient of 20-100% ethyl acetate (with 2% acetic acid) in hexanes. Appropriate fractions are combined and concentrated under vacuum, and the resulting solid is further washed with a mixture of ethyl acetate:hexanes to provide the desired compound. MS (ESI) [M+H+]+=538.0.

Quelle