Reaktion #42019

Reaktionsgleichung

hydrochloric-acid

dibutyl phosphite

acetone

→

dibutyl(1-hydroxy-1-methylethyl)phosphonate

Ausbeute 91.7%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeNext, into a two-liter four-necked flask provided with a stirrer
2. 2
   workup.ADDITIONmixed solution at 40° C.
3. 3
   workup.WAITin an hour
4. 4
   workup.STIRRINGThe mixed solution was further stirred for 1 hour at the same temperature (40° C.)
5. 5
   Sonstigethe reaction
6. 6
   SonstigeThereafter, the resulting reaction solution
7. 7
   Waschenwas washed with a 1% dilute hydrochloric acid aqueous solution
8. 8
   Waschena saturated sodium carbonate aqueous solution successively and rinsed with water twice
9. 9
   Sonstigeto remove the triethylamine
10. 10
    Sonstigewater was recovered under a reduced pressure of about 2.7 kPa
11. 11
    Sonstigeto remove the low-boiling point portions

Vorschrift

Next, into a two-liter four-necked flask provided with a stirrer, a thermometer, a dropping device, a hydrochloric-acid-recovering device and a condenser, 213.4 g (1.1 moles) of dibutyl phosphite, 5.6 g (0.06 moles) of triethylamine and 1.9 g (0.020 moles) of magnesium chloride were fed. While stirring the resulting mixed solution at 40° C., 70.2 g (1.2 moles) of acetone was added thereto in an hour. The mixed solution was further stirred for 1 hour at the same temperature (40° C.) to complete the reaction. Thereafter, the resulting reaction solution was washed with a 1% dilute hydrochloric acid aqueous solution and a saturated sodium carbonate aqueous solution successively and rinsed with water twice to remove the triethylamine and the magnesium chloride. Then, while heating the reaction mixture to 80° C., water was recovered under a reduced pressure of about 2.7 kPa. Further, nitrogen topping was carried out under the same conditions to remove the low-boiling point portions, thereby obtaining 254.6 g of dibutyl(1-hydroxy-1-methylethyl)phosphonate (raw material 2).

Quelle