反应详情

To a stirring solution of 340 mg (0.80 mmol) of 2-(2,4-dioxo-5-thiophen-3-yl-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl)-N-isopropyl-N-(4-methoxy-phenyl)-acetamide, prepared as in Part A, in 10 mL DMF at 0° C. is added 1.93 mL (0.96 mmol, 1.2 equiv) of NaN(TMS)2 in toluene. The resulting solution is stirred 5 min and 299 mg (0.96 mmol, 1.2 equiv) of 3-bromomethyl-1-tert-butoxycarbonyl-1H-indazole is added. The resulting solution is stirred 4.5 h, poured into 100 mL Et2O/EtOAc (1:1), washed with H2O (2×50 mL). The organic layer is separated, dried (MgSO4), and the solvents removed in vacuo to afford 590 mg of the crude title compound: low resolution MS (FAB) m/e 694 (MH+).

1. stirringThe resulting solution is stirred 4.5 h
2. washwashed with H2O (2×50 mL)
3. customThe organic layer is separated
4. dry with materialdried (MgSO4)
5. customthe solvents removed in vacuo