反应详情

To a mixture of 4.9 g (47 mmol) of thiocarbohydrazide and 9.8 g (47 mmol) of 4-nitrophenylbutanoic acid in 30 mL of toluene was added 0.8 g (4.7 mmol) of 3-nitrobenzeneboronic acid. The mixture was heated at reflux for 24 hr. The reaction was cooled and the reaction mixture was allowed to settle. The supernatant liquid was decanted. To the residual solid was added 50 mL of acetonitrile. The mixture was stirred for 30 minutes. The solid was collected, rinsed with 10 mL of acetonitrile and dried in vacuo to yield 8.5 g (65.4%) of the desired product as a white sandy material. All the analytical data confirmed the assigned structure.

1. temperatureThe mixture was heated
2. temperatureat reflux for 24 hr
3. temperatureThe reaction was cooled
4. customThe supernatant liquid was decanted
5. additionTo the residual solid was added 50 mL of acetonitrile
6. customThe solid was collected
7. washrinsed with 10 mL of acetonitrile
8. customdried in vacuo