反应详情

A sol. of compound D4 (7.76 mmol, 4.86 g) in CH2Cl2 (63 mL) was treated with DMAP (1.94 mmol, 0.27 mg), HOBt (9.31 mmol, 1.26 g), EDC.HCl (19.40 mmol, 3.72 g), and DIPEA (31.04 mmol, 5.31 mL). After 30 min at rt, cyclopropyl-(3-methoxy-2-methylbenzyl)amine (prepared by reductive amination from 3-methoxy-2-methylbenzaldehyde, Comins, D. L.; Brown, J. D., J. Org. Chem., 1989, 54, 3730 and cyclopropylamine, 23.28 mmol, 4.45 g) was added and the mixture was stirred for 4 days at rt. The reaction was then diluted with CH2Cl2 (140 mL), washed with aq. 1M HCl (2×100 mL), dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (EtOAc/heptane 30:70) yielded the title compound (0.48 g, 42%). LC-MS: tR=1.27 min; ES+: 799.56.

1. washwashed with aq. 1M HCl (2×100 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customthe solvents were removed under reduced pressure
5. customPurification of the residue by FC (EtOAc/heptane 30:70)