反应详情

After dissolving 7-benzyloxy-6-cyano-4-(1H-indol-5-yloxy)quinoline (3 g, 76.642 mmol) in tetrahydrofuran (250 ml), 10% palladium carbon powder (500 mg, wet) was added and the mixture was stirred for 11 hours at room temperature under a hydrogen atmosphere. After further adding 10% palladium carbon powder (300 mg, wet) and stirring the mixture for 9 hours at room temperature under a hydrogen atmosphere, additional 10% palladium carbon powder (200 mg, wet) was added and the mixture was stirred for 5 hours at room temperature under a hydrogen atmosphere. The solvent was distilled off, washing was performed with ethanol, and then the filtrate was distilled off under reduced pressure. The obtained crystals were suspended in ethanol and diluted with hexane, and the crystals were filtered out, washed with hexane:ethanol=3:1 and dried by aspiration to obtain the title compound (1.82 g, 6.0402 mmol, 79.12%) as light yellow crystals.

1. additionwas added
2. stirringstirring the mixture for 9 hours at room temperature under a hydrogen atmosphere
3. stirringthe mixture was stirred for 5 hours at room temperature under a hydrogen atmosphere
4. distillationThe solvent was distilled off
5. washwashing
6. distillationthe filtrate was distilled off under reduced pressure
7. additiondiluted with hexane
8. filtrationthe crystals were filtered out
9. washwashed with hexane
10. dry with materialethanol=3:1 and dried by aspiration