反应详情

Sodium hydride (60% in mineral oil, 18 mg, 0.74 mmol) was added to a solution of 6-methoxy-m-toluensulfonyl chloride (98.3 mg, 0.445 mmol) and tert-butyl 10-chloro-1-methyl-1,3,4,8-tetrahydro-2H-[1,4]oxazepino[6,7-e]indole-2-carboxylate (Intermediate 43, 50.0 mg, 0.148 mmol) in DMF (2 mL) at room temperature. The mixture was stirred for 15 minutes before water (5 mL) was added and the aqueous layer was extracted with DCM. Most of the organic solvents were evaporated and the residue was dissolved in DCM (1 mL) and TFA (2 mL) was added. The reaction mixture was stirred at room temperature for 30 minutes. Solvents were evaporated and the crude product was purified by preparative HPLC (Xterra C18, 10 mM NH4HCO3 (pH 10) —CH3CN) to give the title compound as a white solid (16.8 mg). MS m/z 421 [M+H]+.

1. additionwas added
2. extractionthe aqueous layer was extracted with DCM
3. customMost of the organic solvents were evaporated
4. dissolutionthe residue was dissolved in DCM (1 mL)
5. additionTFA (2 mL) was added
6. customSolvents were evaporated
7. customthe crude product was purified by preparative HPLC (Xterra C18, 10 mM NH4HCO3 (pH 10) —CH3CN)