反应详情

温度

0 °C

To a suspension of 2-(2-isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-8-carboxylic acid methyl ester (778 mg, 2.1 mmol) in THF (20 mL) at −78° C. under nitrogen was added dropwise diisobutyl aluminium hydride (1.5M in toluene, 4.2 mL, 6.3 mmol) and the reaction mixture was stirred at 0° C. for 2 hours. MeOH (10 mL) was added cautiously followed by an aqueous 1M potassium sodium tartrate solution (7 mL) at RT. The mixture was concentrated in vacuo to remove organic solvent and the aqueous phase was extracted with DCM (×3). The combined organic extracts were dried (MgSO4) and concentrated in vacuo to give the title compound as an off-white solid (713 mg, 99%). LCMS: RT=4.14 min, [M+H]+=343

1. concentrationThe mixture was concentrated in vacuo
2. customto remove organic solvent
3. extractionthe aqueous phase was extracted with DCM (×3)
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. concentrationconcentrated in vacuo