反応 #366703
ord-1a6abe78dbe34eff845943632c9e6d8d
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他was kept below 50° C
- 2ろ過the precipitated product collected by filtration
- 3その他The crude product was purified by chromatography on silica eluting with methylene chloride/hexane progressing
- 4温度through increasingly polar mixtures to methanol/methylene chloride (1/19)
実験手順
A mixture of concentrated nitric acid (6 ml) and concentrated sulphuric acid (6 ml) was added slowly to a solution of 4-fluoro-2-methylphenyl methyl carbonate (11.34 g, 62 mmol) in concentrated sulphuric acid (6 ml) such that the temperature of the reaction mixture was kept below 50° C. The mixture was stirred for 2 hours, then ice/water was added and the precipitated product collected by filtration. The crude product was purified by chromatography on silica eluting with methylene chloride/hexane progressing through increasingly polar mixtures to methanol/methylene chloride (1/19) to give 4-fluoro-2-methyl-5-nitrophenol (2.5 g, 22%) as a solid.