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 solution of 4-chloromethyl-2-(2-methyl-[1,3]dioxolan-2-yl)-thiazole (231 mg, 1.05 mmol) in DMF (1.5 mL) was added to a solution of 4-nitro-2H-[1,2,3]triazole (100 mg, 0.88 mmol) in DMF (1.5 mL) pre-treated for 30 min with DIPEA (0.30 mL, 1.75 mmol) and the reaction mixture was stirred for 48 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 NaSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (6:4 hept-EA) gave the title compound as a pale yellow oil: TLC:rf (6:4 hept-EA)=0.33. LC-MS-conditions 02: tR=0.90 min, [M+H]+=298.23.

1. additionwere added
2. extractionThe aq. layer was extracted with EA (10 mL)
3. dry with materialextracts were dried over NaSO4
4. filtrationfiltered
5. customthe solvents were removed under reduced pressure
6. customPurification of the residue by FC (6:4 hept-EA)