تفاعل #57404

معادلة التفاعل

ether

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

Sodium hydroxide

hydrochloric acid

→

title compound

المردود 57.6%

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

المردود 57.6%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONThe addition
2. 2
   workup.STIRRINGthe solution was further stirred for 20 min
3. 3
   درجة الحرارةThe reaction solution was cooled to 55° C.
4. 4
   أخرىwhich resulted in precipitation of a large amount of crystals
5. 5
   workup.STIRRINGUnder stirring
6. 6
   أخرىby leaving it for about 1 hr
7. 7
   workup.STIRRINGthe mixture was stirred
8. 8
   ترشيحfiltered
9. 9
   غسيلThe obtained crystals were washed alternately with water and ether
10. 10
    أخرىdried

الإجراء التجريبي

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%).

المصدر