反应详情

To a solution of N-Boc-L-pipecolinic acid (200 mg, 0.87 mmol) in DMF (3.5 mL) was added TBTU (336 mg, 1.05 mmol), ammonium chloride (93 mg, 1.74 mmol) then DIPEA (182 μL, 1.05 mmol) and the reaction stirred for 16 h. The mixture was partitioned between ethyl acetate (2×30 mL) and water (30 mL), and the organics combined before being washed with 1M sodium hydroxide (3×30 mL) and brine (3×30 mL). The organic solution was dried (MgSO4) and solvent removed in vacuo to give the title compound as a white solid. δH (d6 DMSO): 7.23 (1H, s), 6.97 (1H, s), 4.56-4.39 (1H, br m), 3.43-3.74 (1H, d), 3.14-2.90 (1H, br m), 2.09-2.00 (1H, d), 1.63-1.47 (3H, m), 1.30-1.17 (2H, m).

1. customThe mixture was partitioned between ethyl acetate (2×30 mL) and water (30 mL)
2. washbefore being washed with 1M sodium hydroxide (3×30 mL) and brine (3×30 mL)
3. dry with materialThe organic solution was dried (MgSO4) and solvent
4. customremoved in vacuo