反应详情

温度

110 °C

In a microwave vial, 3-methyl-3,4-dihydro-2H-chromen-5-ol (Intermediate 117, 53 mg), potassium carbonate (134 mg, 0.968 mmol) and 2-chloro-5-nitropyridine (51.2 mg, 0.323 mmol) were dissolved in N,N-dimethylformamide (2 ml) to give a light brown solution. The reaction vessel was sealed and heated in Biotage Initiator at 110° C. for 1 hour. After cooling, the reaction mixture was quenched with 5 ml of water and diluted with 10 ml of Et2O. Phases were separated by a separating funnel. The aqueous phase was extracted with 3×10 ml of Et2O. The collected organic phase were dried using a hydrophobic frit and evaporated under vacuum to give the title compound as a brown oil (181 mg).

1. customto give a light brown solution
2. customThe reaction vessel was sealed
3. temperatureAfter cooling
4. customthe reaction mixture was quenched with 5 ml of water
5. additiondiluted with 10 ml of Et2O
6. customPhases were separated by a separating funnel
7. extractionThe aqueous phase was extracted with 3×10 ml of Et2O
8. customThe collected organic phase were dried
9. customevaporated under vacuum