反应详情

温度

30 °C

2.0 Grams (0.00855 mole) of 1,3-dimethyl-5-phenoxypyrazole-4-carbaldehyde oxime was dissolved in 20 ml of dimethyl sulfoxide, and after adding 0.65 g (0.0116 mole) of powdery potassium hydroxide, the resulting mixture was stirred at 30° C. for 30 minutes. To this solution was added 2.32 g (0.00855 mole) of tert-butyl 4-bromomethylbenzoate, and reaction was carried out at from 50° to 60° C. for 1 hour. After completion of the reaction, water was added to the reaction solution which was then extracted with ethyl acetate. The ethyl acetate extract was washed with water and dried, and ethyl acetate was removed by evaporation to obtain crude crystals. The crystals were recrystallized from methanol to obtain 2.4 g of the desired compound.

1. additionTo this solution was added
2. waitwas carried out at from 50° to 60° C. for 1 hour
3. additionwas added to the reaction solution which
4. extractionwas then extracted with ethyl acetate
5. extractionThe ethyl acetate extract
6. washwas washed with water
7. customdried
8. customethyl acetate was removed by evaporation
9. customto obtain crude crystals
10. customThe crystals were recrystallized from methanol