تفاعل #318646

معادلة التفاعل

acryloyl chloride

water

p-hydroxybenzophenone

sodium hydroxide

→

oily product

المردود 84.5%

para-acryloxybenzophenone

المردود 84.5%

المذيبات

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   أخرىA three-neck round-bottom flask fitted with an addition funnel
2. 2
   درجة الحرارةThe flask was cooled in an ice bath to 8°-10° C.
3. 3
   أخرىat 8°-10° C
4. 4
   workup.ADDITIONWhen the addition
5. 5
   workup.DISSOLUTIONto dissolve
6. 6
   أخرىthe product of the reaction
7. 7
   أخرىThe ether layer was separated from the water layer
8. 8
   غسيلwashed twice with 3% sodium hydroxide and twice with water
9. 9
   تجفيفThe solution was dried over magnesium sulfate
10. 10
    ترشيحfiltered

الإجراء التجريبي

A three-neck round-bottom flask fitted with an addition funnel, thermometer and a mechanical stirrer was charged with 100 ml of water, 40 g (0.20M) of p-hydroxybenzophenone and 8.8 g of sodium hydroxide. The flask was cooled in an ice bath to 8°-10° C., then 20 g (0.22) of acryloyl chloride were added dropwise while holding the temperature at 8°-10° C. When the addition was complete, the reaction mixture was stirred for an additional half hour. Then 150 ml of diethyl ether was added to dissolve the product of the reaction. The ether layer was separated from the water layer and washed twice with 3% sodium hydroxide and twice with water. The solution was dried over magnesium sulfate, filtered and stripped. An amount of 43.0 g of an oily product was obtained and purified by recrystallization from absolute ethanol, from which an amount of about 34.7 g of white crystalline product was isolated.

المصدر