반응 #42020

반응 방정식

hydrochloric-acid

dibutylphosphite

methyl isobutyl ketone

→

dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate

수율 92.3%

반응 조건

후처리

1. 1
   기타Into a two-liter four-necked flask provided with a stirrer
2. 2
   workup.ADDITIONmixed solution at 25° C.
3. 3
   workup.ADDITIONThe resulting mixed solution
4. 4
   workup.STIRRINGwas further stirred for 1 hour at the same temperature (25° C.)
5. 5
   기타the reaction
6. 6
   세척Thereafter, the mixed solution was washed
7. 7
   기타to remove the low-boiling point portions
8. 8
   기타as in (synthesis of raw material 2) of Example 1
9. 9
   기타thus, the triethylamine and the magnesium chloride was removed from the mixed solution

실험 절차

Into a two-liter four-necked flask provided with a stirrer, a thermometer, dropping device, a hydrochloric-acid-recovering device and a condenser, 213.4 g (1.1 moles) of dibutylphosphite, 5.6 g (0.06 moles) of triethylamine and 1.05 g (0.011 moles) of magnesium chloride were fed. While stirring the resulting mixed solution at 25° C., 120.0 g (1.2 moles) of methyl isobutyl ketone (MIBK) was added thereto in 1 hour. The resulting mixed solution was further stirred for 1 hour at the same temperature (25° C.) to complete the reaction. Thereafter, the mixed solution was washed to remove the low-boiling point portions, as in (synthesis of raw material 2) of Example 1, and thus, the triethylamine and the magnesium chloride was removed from the mixed solution, to obtain 298.8 g of dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate (raw material 3).

출처