Reacción #8800

Ecuación de reacción

product

Methyl-(4-methyl-piperidin-3-yl)-(7H-Pyrrolo[2,3-d]pyrimidin-4-yl)-amine

acetylchloride

→

title compound

Rendimiento 15.0%

1-{4-Methyl-3-[methyl-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-amino]-piperidin-1-yl}-ethanone

Rendimiento 15.0%

Disolventes

dichloromethane pyridine

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe reaction mixture was then partitioned between dichloromethane and saturated sodium bicarbonate (NaHCO3)
2. 2
   LavadoThe organic layer was washed again with saturated NaHCO3, dried-over sodium sulfate
3. 3
   Concentraciónconcentrated to dryness in vacuo
4. 4
   OtroThe residue was purified by preparative thin layer chromatography (PTLC) (silica; 4% methanol in dichloromethane)

Procedimiento

To a stirred solution of the product from Method C (0.03 grams, 0.114 mmol) dissolved in 5 mL of 10:1 dichloromethane/pyridine was added (0.018 grams, 0.228 mmol) of acetylchloride and the resulting mixture stirred at room temperature for 18 hours. The reaction mixture was then partitioned between dichloromethane and saturated sodium bicarbonate (NaHCO3). The organic layer was washed again with saturated NaHCO3, dried-over sodium sulfate and concentrated to dryness in vacuo. The residue was purified by preparative thin layer chromatography (PTLC) (silica; 4% methanol in dichloromethane) affording 0.005 mg (15%) of the title compound as a colorless oil. LRMS: 288.1 (M+1).

Fuente