反应详情

温度

80 °C

To a suspension of Fe (1.1 g, 19.6 mmole), NH4Cl (1.5 g, 28 mmole) in a mixture of ethanol/water (30 ml/7 ml) at 80° C. was added a mixture of 5-Nitro-2,3-dihydro-isoindol-1-one (1 g, 5.6 mmole) in 10 ml ethanol. The reaction mixture was stirred at 80° C. for 2 hours. Mixture was cooled down, filtered off, solid was washed with 50 ml ethanol. The filtrate was concentrated, taken into 50 ml ethylacetate, washed with 20 ml water. Organic layer was dried over Na2SO4, filtered and concentrated to give about 900 mg crude. Trituration with methyl t-butylether gave 400 mg pure product, 48% yield.

1. additionwas added
2. temperatureMixture was cooled down
3. filtrationfiltered off
4. washsolid was washed with 50 ml ethanol
5. concentrationThe filtrate was concentrated
6. washwashed with 20 ml water
7. dry with materialOrganic layer was dried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated
10. customto give about 900 mg crude