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 4-benzyloxybutyric acid (246 mg, 1.27 mmol), pyrrolidine (0.13 mL, 1.52 mmol), EDC.HCl (493 mg, 2.53 mmol), HOBt (262 mg, 1.90 mL) and DIPEA (0.65 mL, 3.80 mmol) in CH2Cl2 (10 mL) was heated at rt until completion of the reaction. Water was added, the layers separated and the aq. layer extracted with CH2Cl2 (2×). The combined org. extracts were washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure. The crude residue was purified by FC (hept-EA, 1:0→0:1) to give 4-(benzyloxy)-1-(pyrrolidin-1-yl)butan-1-one as a colorless oil. LC-MS-conditions 08: tR=0.77 min; [M+H]+=247.95.

1. customthe layers separated
2. extractionthe aq. layer extracted with CH2Cl2 (2×)
3. washextracts were washed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude residue was purified by FC (hept-EA, 1:0→0:1)