反应详情

TBTU (4.93 g, 15.4 mmol) was added to a rt solution of 5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid A-1-2 (2.40 mg, 11.8 mmol) and DIPEA (8.09 mL, 47.2 mmol) in DCM (24 mL) and after stirring for 15 min, (S)-methyl azetidine-2-carboxylate HCl (2.03 g, 13 mmol) was added and the resulting mixture was stirred at rt for 1 h. The rxn mixture was diluted with DCM and water, the layers were separated and the aq. layer was extracted with DCM (1×). The combined org. extracts were washed with brine, dried (MgSO4), filtered and concentrated in vacuo. The crude was purified by FC (EtOAc/hept 5:1) to obtain the title compound A-2-1 as a white solid. LC-MS A: tR=0.70 min; [M+H]+=301.18.

1. customthe layers were separated
2. extractionthe aq. layer was extracted with DCM (1×)
3. washextracts were washed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude was purified by FC (EtOAc/hept 5:1)