反应详情

温度

47.5 °C

At 20° C., 73.5 g (0.88 mol) of methoxyamine hydrochloride are added to a solution of 80.0 g (0.44 mol) of o-hydroxy-ω-nitroacetophenone in 500 ml of methanol, and the mixture is stirred at 45 to 50° C. for 8 to 12 hours. The solution is cooled to 20° C., poured into 1 l of ice-water and stirred for one hour. The crystalline product is filtered off and washed with 500 ml of water a little at a time and dried at 40° C. in a vacuum drying cabinet. 72 g (74.6% of theory) of 1-(2-hydroxyphenyl)-2-nitro-ethanone O-methyl-oxime are obtained as a mixture of stereoisomers.

1. temperatureThe solution is cooled to 20° C.
2. stirringstirred for one hour
3. filtrationThe crystalline product is filtered off
4. washwashed with 500 ml of water a little at a time
5. customdried at 40° C. in a vacuum
6. customdrying cabinet