反応 #57407

反応方程式

Sodium hydroxide

2-chloro-5,5-dimethyl-4-(2-naphthyl)-1,3,2-dioxaphosphorinane-2-one

hydrochloric acid

→

title compound

収率 93.2%

2-Hydroxy-5,5-dimethyl-4-(2-naphthyl)-1,3,2-dioxaphosphorinane 2-oxide

収率 93.2%

溶媒

water

反応条件

後処理

1. 1
   workup.STIRRINGThe solution was stirred at the same temperature for 20 min
2. 2
   温度the reaction solution was cooled to 45° C
3. 3
   workup.STIRRINGThe solution was stirred at 15° C. for 30 min
4. 4
   ろ過The crystals were collected by filtration
5. 5
   洗浄washed with water
6. 6
   乾燥ether, and dried under reduced pressure at 60° C.

実験手順

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%).

出典