反应详情

温度

15 °C

To 243 grams (1.76 moles) of diethyl phosphite stirred under nitrogen and protected by a drying tube was added a solution of sodium ethoxide prepared from 5.07 grams (0.22 mole) of sodium in 100 ml of anhydrous ethanol. Methyl vinyl ketone, 112 grams (1.60 moles), was then added at such a rate as to keep the temperature at 35°-40° C. The addition required about one hour. The reaction mixture was stirred for one-half hour after the addition was completed and was stripped to dryness in vacuo at 60° C./16 mm. The residue was taken up in 600 ml of chloroform, and the solution cooled to 15° C. and washed successively with dilute acid, water and saturated sodium chloride solution. After drying, the chloroform solution was distilled to yield 112 grams of diethyl 3-oxobutylphosphonate as a colorless liquid, B.P. 106° C./0.05 mm, nD 25 1.4340. VPC indicated that the product was 90% pure.

1. customprotected by a drying tube
2. customat 35°-40° C
3. additionThe addition required about one hour
4. additionafter the addition
5. customwas stripped to dryness in vacuo at 60° C.
6. washwashed successively
7. additionwith dilute acid, water and saturated sodium chloride solution
8. customAfter drying
9. distillationthe chloroform solution was distilled