反应详情

A mixture of m-nitrophenylglycine (58.0 g, 0.296 mol), MgO (23.92 g, 0.6 mol) and t-butoxylcarbonyl azide (85.2 g, 0.6 mol) in 50% aqueous dioxane (700 ml) was heated at 45° for 17 hours. The reaction was cooled, water (750 ml) was added, and the mixture was filtered. The filtrate was washed with ether (1000 ml), acidified to pH 3 with 40% H3PO4, and extracted with ethyl acetate. The dried extracts were evaporated to give α-t-butoxycarbonylamino-m-nitrophenylacetic acid (70.3 g).

1. temperaturewas heated at 45° for 17 hours
2. temperatureThe reaction was cooled
3. filtrationthe mixture was filtered
4. washThe filtrate was washed with ether (1000 ml)
5. extractionextracted with ethyl acetate
6. customThe dried extracts were evaporated