반응 #57404

반응 방정식

ether

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

Sodium hydroxide

hydrochloric acid

→

title compound

수율 57.6%

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

수율 57.6%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONThe addition
2. 2
   workup.STIRRINGthe solution was further stirred for 20 min
3. 3
   온도The reaction solution was cooled to 55° C.
4. 4
   기타which resulted in precipitation of a large amount of crystals
5. 5
   workup.STIRRINGUnder stirring
6. 6
   기타by leaving it for about 1 hr
7. 7
   workup.STIRRINGthe mixture was stirred
8. 8
   여과filtered
9. 9
   세척The obtained crystals were washed alternately with water and ether
10. 10
    기타dried

실험 절차

Sodium hydroxide (29.4 g, 0.735 mol) was dissolved in water (300 ml). To the solution was added 2-chloro-5,5-dimethyl-4-(1-naphthyl)-1,3,2-dioxaphosphorinane 2-oxide (76.1 g, 0.245 mol) little by little, with stirring and heating at 100° C. The addition was completed for 35 min, and the solution was further stirred for 20 min. The reaction solution was cooled to 55° C., which resulted in precipitation of a large amount of crystals. Under stirring, concentrated hydrochloric acid (73 ml) was added to the mixture to adjust the mixture to acidic, and the mixture solidified and turned into powder by leaving it for about 1 hr. To the powder was added ether (100 ml), and the mixture was stirred and filtered. The obtained crystals were washed alternately with water and ether and dried to give the title compound as pale ocher crystals having the melting point of 216 to 217° C. (41.23 g, yield 57.6%).

출처