反应详情

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 2-[4-(2-methyl-[1,3]dioxolan-2-yl)-thiazol-2-ylmethyl]-4-nitro-2H-[1,2,3]triazole (2.360 g, 7.94 mmol) in THF (40.0 mL) was treated with 1N HCl (21.4 mL, 21.4 mmol) and the reaction mixture was stirred at rt overnight. The reaction mixture was neutralized with 1N NaOH. The aq. layer was extracted twice with EA (20 mL) and the combined org. extracts were dried over MgSO4, 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 yellow solid: TLC:rf (6:4 hept-EA)=0.29. LC-MS-conditions 02: tR=0.81 min, [M+H]+=254.35.

1. extractionThe aq. layer was extracted twice with EA (20 mL)
2. dry with materialextracts were dried over MgSO4
3. filtrationfiltered
4. customthe solvents were removed under reduced pressure
5. customPurification of the residue by FC (6:4 hept-EA)