反应详情

温度

50 °C

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a suspension of 4-nitro-2H-[1,2,3]triazole (114 mg, 1.00 mmol) in DMF (1.0 mL) was treated with DIPEA (0.34 mL, 2.00 mmol). After 30 min, a solution of 6-bromo-hexan-2-one (179 mg, 1.00 mmol) in DMF (1.0 mL) was added and the reaction mixture was stirred for 24 h at 50° C. Water (10 mL), followed by EA (10 mL) were added. The aq. layer was extracted with EA (10 mL) and the combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (2:1 hept-EA) gave the title compound as a yellow oil: TLC:rf (2:1 hept-EA)=0.26. LC-MS-conditions 02: tR=0.86 min.

1. additionwere added
2. extractionThe aq. layer was extracted with EA (10 mL)
3. dry with materialextracts were dried over Na2SO4
4. filtrationfiltered
5. customthe solvents were removed under reduced pressure
6. customPurification of the residue by FC (2:1 hept-EA)