反应详情

To a suspension of 7-amino-3,4-dihydro-2H-isoquinolin-1-one (8.1 g, 50 mmol) in conc. HCl (100 mL) cooled in an ice-H2O bath was added a solution of NaNO2 (3.45 g, 50 mmol) in H2O dropwise at such a rate that the reaction mixture never rose above 5° C. After stirring for 30 min, to the resulting mixture was added a solution of SnCl2.2H2O (22.5 g, 0.1 mol) in conc. HCl (150 mL) dropwise at 0° C. in an ice-H2O bath. The resulting mixture was stirred for another 2 h at 0° C. The precipitate was collected by suction, washed with ether to afford 7-hydrazino-3,4-dihydro-2H-isoquinolin-1-one (8.3 g), which was used for the next reaction without further purification.

1. temperaturecooled in an ice-H2O bath
2. stirringThe resulting mixture was stirred for another 2 h at 0° C
3. customThe precipitate was collected by suction
4. washwashed with ether