تفاعل #613987

معادلة التفاعل

3-hydroxy-2-butanone

triethylamine

methacryloyl chloride

→

3-oxobutane-2-yl methacrylate

المردود 53.1%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىIn a 2 L four-necked flask subjected
2. 2
   درجة الحرارةa stirrer, a thermometer and a Dimroth cooling tube
3. 3
   درجة الحرارةWhile the solution was cooled to about 5° C.
4. 4
   workup.STIRRINGunder stirring
5. 5
   workup.STIRRINGfurther stirred for 30 minutes
6. 6
   workup.ADDITIONafter completion of the dropwise addition
7. 7
   أخرىa reaction
8. 8
   أخرىThe resulting reaction mixture
9. 9
   غسيلwas washed with 1 N-hydrochloric acid
10. 10
    تجفيفa 10% sodium carbonate aqueous solution and saturated brine at room temperature, dried over anhydrous magnesium sulfate
11. 11
    أخرىseparated by filtration
12. 12
    أخرىto obtain
13. 13
    أخرىa reaction crude liquid
14. 14
    أخرىThe solvent of the reaction crude liquid
15. 15
    workup.DISTILLATIONwas distilled off
16. 16
    أخرىan evaporator, 80 mg of p-methoxyphenol
17. 17
    workup.ADDITIONwas added
18. 18
    workup.DISTILLATIONthe resulting solution was distilled under reduced pressure

الإجراء التجريبي

In a 2 L four-necked flask subjected replacement with nitrogen, 150 g of 3-hydroxy-2-butanone (made by Tokyo Chemical Industry Co., Ltd., purity: 95.0% or more) was put, and dissolved in 750 g of methylene chloride, and a stirrer, a thermometer and a Dimroth cooling tube were connected thereto. After the solution was stirred and cooled to about 5° C., 190 g of triethylamine and 80 mg of p-methoxyphenol were added thereto. While the solution was cooled to about 5° C. under stirring, 178 g of methacryloyl chloride was slowly added dropwise thereto over 4 hours, and further stirred for 30 minutes after completion of the dropwise addition to allow a reaction. The resulting reaction mixture was washed with 1 N-hydrochloric acid, a 10% sodium carbonate aqueous solution and saturated brine at room temperature, dried over anhydrous magnesium sulfate and separated by filtration to obtain a reaction crude liquid. The solvent of the reaction crude liquid was distilled off using an evaporator, 80 mg of p-methoxyphenol was added thereto and the resulting solution was distilled under reduced pressure to give 141 g of 3-oxobutane-2-yl methacrylate of 96.5% GC purity (yield: 53.1% based on 3-hydroxy-2-butanone).

المصدر