反应 #72693

反应方程式

product

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

acetylchloride

→

title compound

收率 15.0%

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

收率 15.0%

溶剂

dichloromethane pyridine

反应条件

后处理

1. 1
   其他The reaction mixture was then partitioned between dichloromethane and saturated sodium bicarbonate (NaHCO3)
2. 2
   洗涤The organic layer was washed again with saturated NaHCO3
3. 3
   干燥dried over sodium sulfate
4. 4
   浓缩concentrated to dryness in vacuo
5. 5
   其他The residue was purified by preparative thin layer chromatography (PTLC) (silica; 4% methanol in dichloromethane)

实验过程

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).

来源