反应详情

The formyl compound (4.3 g., 0.01 mole), N,O-bis (trifluoroacetyl)hydroxylamine (3.6 g., 0.016 mole) and dry pyridine (2.6 ml. 0.032 mole) were mixed in benzene (75 ml) and heated under reflux for 2 hours. After cooling the benzene solution was washed with water (2×50 ml), dried over magnesium sulphate monohydrate and evaporated in vacuo to give an oil which slowly crystallised. This product was further purified by silica gel chromatography and recrystallisation from a small volume of ethyl acetate to give the title compound, yield 2.5 g., m.p. 136° C.

1. temperatureheated
2. temperatureunder reflux for 2 hours
3. washwas washed with water (2×50 ml)
4. dry with materialdried over magnesium sulphate monohydrate
5. customevaporated in vacuo
6. customto give an oil which
7. customslowly crystallised
8. customThis product was further purified by silica gel chromatography and recrystallisation from a small volume of ethyl acetate