反应详情

温度

101 °C

Sodium hydroxide (14.9 g, 0.373 mol) was dissolved in water (150 ml). To this solution was added little by little 2-chloro-5,5-dimethyl-4-(2-naphthyl)-1,3,2-dioxaphosphorinane-2-one (38.6 g, 0.124 mol) with heating to 100 to 102° C. and stirring for 30 min. The solution was stirred at the same temperature for 20 min, and the reaction solution was cooled to 45° C. Concentrated hydrochloric acid (37 ml) was added thereto to adjust the solution to acidic. The solution was stirred at 15° C. for 30 min. The crystals were collected by filtration, washed with water and then ether, and dried under reduced pressure at 60° C. to give the title compound as pale ocher crystals having the melting point of 237 to 238° C. (33.87 g, yield 93.2%).

1. stirringThe solution was stirred at the same temperature for 20 min
2. temperaturethe reaction solution was cooled to 45° C
3. stirringThe solution was stirred at 15° C. for 30 min
4. filtrationThe crystals were collected by filtration
5. washwashed with water
6. dry with materialether, and dried under reduced pressure at 60° C.