反应详情

温度

95 °C

tert-Butyl 2-fluoro-4-nitrobenzoate (24.2 g, 0.100 mol) was added to a warm (95° C.) solution of ammonium chloride (53.5 g, 1.00 mol), dissolved in ethanol (300 ml) and water (150 ml). Iron powder (325 mesh, 16.8 g, 0.300 mol) was added with stirring in small portions over ca. 1 h. The reaction mixture was stirred and heated at 95° C. for another 30 minutes and then filtered while still warm. The filter cake was washed thoroughly with excess ethanol. The filtrate and washings were diluted with water (1 L) and extracted with ether (3×150 ml). Combined ether extracts were washed with water and brine, dried (MgSO4), and evaporated to give the product as an off-white solid (21.1 g, 98%); mp 100-101° C. 1H NMR.

1. stirringThe reaction mixture was stirred
2. filtrationfiltered
3. temperaturewhile still warm
4. washThe filter cake was washed thoroughly with excess ethanol
5. additionThe filtrate and washings were diluted with water (1 L)
6. extractionextracted with ether (3×150 ml)
7. washCombined ether extracts were washed with water and brine
8. dry with materialdried (MgSO4)
9. customevaporated