反应详情

Phenyl N-(4-(1-(methylamino)carbonyl-1H-5-indolyloxy)-2-pyridyl)-N-(phenoxycarbonyl)carbamate (15.5 g, 29.7 mmol) synthesized in Production example 5-2 was dissolved in dimethylformamide (180 ml); 4-piperidinopiperidine (20.0 g, 119 mmol) was added thereto; and the reaction mixture was stirred at room temperature for 9 hours. The reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine and concentrated to about 100 ml. The residue was allowed to be kept cool at 5° C. overnight to precipitate crystals. The crystals were filtered off and washed with ethyl acetate to yield the title compound (4.0 g, 8.4 mmol, 28%) as white crystals.

1. customThe reaction mixture was partitioned between ethyl acetate and water
2. washThe organic layer was washed with brine
3. concentrationconcentrated to about 100 ml
4. temperatureto be kept cool at 5° C. overnight
5. customto precipitate crystals
6. filtrationThe crystals were filtered off
7. washwashed with ethyl acetate