反应详情

温度

-50 °C

A mixture of 3.00 g of 4-(2,3-dihydro-3-oxo-6-pyridazinyl) benzaldehyde, 6.12 g of β-ethoxyethyltriphneyl phosphonium chloride and 50 ml of N,N-dimethylformamide was cooled to -50° C. and stirred. 20 ml of an N,N-dimethylformamide solution of 5.55 g of potassium tert-butoxide was dropped and the temperature was gradually raised to 0° C. After 2 hours, the temperature was elevated to a room temperature and stirring was conducted for further 10 hours. Iced water was added and the aqueous layer was washed with chloroform. The aqueous layer was adjusted to about pH 3 with hydrochloric acid and deposited solids were collected by filtration. They were recrystallized from 50% hydrous N,N-dimethylformamide to obtain 1.51 g of the above-captioned compound as pale orange powder (yield: 39%).

1. temperaturethe temperature was gradually raised to 0° C
2. customwas elevated to a room temperature
3. stirringstirring
4. waitwas conducted for further 10 hours
5. washthe aqueous layer was washed with chloroform
6. filtrationwere collected by filtration
7. customThey were recrystallized from 50% hydrous N,N-dimethylformamide