反应详情

温度

65 °C

The o-nitrophenoxyacetone is prepared by heating with agitation for five hours at about 65° C. a mixture which consists of 421.6 g (3.006 moles) of o-nitrophenol, 297.8 g (3.09 moles) of chloroacetone, 37.2 g (96%, 0.3615 moles) of sodium bromide, 277.2 g (3.3 moles) of sodium bicarbonate, 21.8 g (0.0647 moles) of aqueous tributylmethylammonium chloride (TBMAC), and 829 g of toluene. There is then added 9.0 g (0.093 mole) of additional chloroacetone to the mixture which is further heated at 65° C. for 2.5 hours (note, sample analysis indicated that the reaction was complete after 1.5 hours). There is then added, 570 g of water and the pH of the mixture is adjusted to 6.5–7 at 55° C. to 60° C. upon addition of 55 g of a 10% HCl solution. The phases are allowed to separate and the aqueous phase is removed.

1. temperatureis further heated at 65° C. for 2.5 hours (note, sample analysis
2. additionThere is then added
3. customto separate
4. customthe aqueous phase is removed