反应详情

A mixture of 2-ethynyl-6-methyl-pyridine (0.08 g, 0.7 mmol), 1-Boc-4-piperidinecarboxaldehyde (0.1 g, 0.47 mmol), CuI (0.001 g, 0.11 mmol) and 33% w/w aqueous dimethylamine (0.077 mL, 0.56 mmol) in water (3 mL) was sonicated for 2 h in a laboratory ultrasonic bath. Afterwards, it was extracted with EtOAc and the combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to give a crude, which was purified by automated flash liquid chromatography (Horizon™-Biotage) eluting with EtOAc—Petroleum Ether 1:1 affording the title product (0.11 g).

1. customwas sonicated for 2 h in a laboratory ultrasonic bath
2. extractionAfterwards, it was extracted with EtOAc
3. washthe combined organic layers were washed with brine
4. customdried on Na2SO4
5. customevaporated to dryness in vacuo
6. customto give a crude, which
7. customwas purified by automated flash liquid chromatography (Horizon™-Biotage)
8. washeluting with EtOAc—Petroleum Ether 1:1 affording the title product (0.11 g)