反应详情

The product from (c) (4.1 g) in 1,2-dichloro-ethane (25 ml) was chilled to -10° C. and concentrated sulphuric acid (25 ml) added. The mixture was stirred and kept at -5° to -10° C. while potassium nitrate (2.3 g) was added in portions over a period of 30 minutes. The mixture was stirred for a further 30 minutes at below 0° C. and then poured on to ice (150 ml). The mixture was extracted with chloroform (150 ml) and the extracts washed with water (100 ml), dried (MgSO4) and evaporated to give 3-fluoro-4-hydroxy-5-nitrobenzotrifluoride as a pale yellow liquid (4.1 g).

1. additionwas added in portions over a period of 30 minutes
2. stirringThe mixture was stirred for a further 30 minutes at below 0° C.
3. extractionThe mixture was extracted with chloroform (150 ml)
4. washthe extracts washed with water (100 ml)
5. dry with materialdried (MgSO4)
6. customevaporated