反应详情

A degassed mixture of the product of Step 3 (6.6 g, 26.0 mmol), 1-methoxyimino-indan-5-boronic acid (5.3 g, 26.0 mmol) and potasium carbonate (28 g, 202 mmol) in ethylene glycol dimethyl ether (150 ml) and water (75 ml) was treated with bis(triphenylphosphine) palladium (II) chloride (1.05 g, 1.5 mmol), then heated under reflux for 6 hours. After cooling to room temperature, the mixture was filtered through celite and the filtrate diluted with water and ethyl acetate. The organic phase was separated, washed with water and brine, dried, concentrated in vacuo and the residue purified by silica gel chromatography eluting with dichloromethane to give the title compound (3.06 g, 35%); MS(ES+) m/e 334/336 [M+H]+.

1. temperatureheated
2. temperatureunder reflux for 6 hours
3. filtrationthe mixture was filtered through celite
4. additionthe filtrate diluted with water and ethyl acetate
5. customThe organic phase was separated
6. washwashed with water and brine
7. customdried
8. concentrationconcentrated in vacuo
9. customthe residue purified by silica gel chromatography
10. washeluting with dichloromethane