반응 #72693

반응 방정식

product

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

acetylchloride

→

title compound

수율 15.0%

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

수율 15.0%

용매

dichloromethane pyridine

반응 조건

후처리

1. 1
   기타The reaction mixture was then partitioned between dichloromethane and saturated sodium bicarbonate (NaHCO3)
2. 2
   세척The organic layer was washed again with saturated NaHCO3
3. 3
   건조dried over sodium sulfate
4. 4
   농축concentrated to dryness in vacuo
5. 5
   기타The residue was purified by preparative thin layer chromatography (PTLC) (silica; 4% methanol in dichloromethane)

실험 절차

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).

출처