反应详情

温度

120 °C

33.2 g of 4-nitrobenzoic acid (200.0 mM), 24.4 g of 1,6-dibromohexane (100.0 mM) and 41.5 g of potassium carbonate (300.0 mM) were suspended in 200 ml of DMF and this mixture was stirred at 120° C. for 2 h. It was then cooled to 60° C., poured onto 600 ml of water and the resulting suspension was stirred for 5 min. The precipitate was filtered off and the still wet cake was refluxed for 1 h in 300 ml of ethanol. It was then cooled to room temperature and filtered. The cake was washed with ethanol and dried to give 40.3 g (96.8 mM, 97%) of 6-[(4-nitrobenzoyl)oxy]hexyl 4-nitrobenzoate as a pale yellow powder.

1. temperatureIt was then cooled to 60° C.
2. stirringthe resulting suspension was stirred for 5 min
3. filtrationThe precipitate was filtered off
4. temperaturethe still wet cake was refluxed for 1 h in 300 ml of ethanol
5. temperatureIt was then cooled to room temperature
6. filtrationfiltered
7. washThe cake was washed with ethanol
8. customdried