反应详情

A mixture of 2-(4-methoxy-5-nitro-pyridin-2-ylmethyl)-isoindole-1,3-dione (0.24 g, 7.7 mmole) and 48% hydrobromic acid (3 mL), is refluxed for 3 hours. The reaction mixture is cooled, evaporated to dryness in vacuo, dissolved in absolute ethanol (25 mL) and 10% Palladium on carbon (100 mg) is added under an inert atmosphere. This is then hydrogenated on a Par apparatus at 45 psi for 2 hours. The reaction mixture is filtered and evaporated to give a brown solid, 60 mg, (23%), MS (ES+): m/z 140.2 (M+H). Used as is for the next step.

1. temperatureis refluxed for 3 hours
2. temperatureThe reaction mixture is cooled
3. customevaporated to dryness in vacuo
4. dissolutiondissolved in absolute ethanol (25 mL)
5. addition10% Palladium on carbon (100 mg) is added under an inert atmosphere
6. filtrationThe reaction mixture is filtered
7. customevaporated
8. customto give a brown solid, 60 mg, (23%), MS (ES+)