تفاعل #555753

معادلة التفاعل

water

4-fluoro-2-(trifluoromethyl)benzonitrile

5,5-dimethyl-hydantoin

K2CO3

→

expected compound

المردود 46.0%

4-(4,4-dimethyl-2,5-dioxoimidazolidin-1-yl)-2-(trifluoromethyl)benzonitrile

المردود 46.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىto be placed in a microwave oven
2. 2
   أخرىUnder magnetic stirring, each tube is irradiated at 140° C. for 20 minutes
3. 3
   أخرىThe reaction masses
4. 4
   استخلاصextracted with AcOEt (2×75 ml)
5. 5
   غسيلwashed with salt water
6. 6
   تجفيفdried over Na2SO4
7. 7
   ترشيحfiltered
8. 8
   تركيزThe filtrate is concentrated under reduced pressure
9. 9
   أخرىthe residue crystallizeds from Et2O (25 ml)
10. 10
    أخرىAfter recrystallization from EtOH (75 ml)
11. 11
    ترشيحthe powder is filtered
12. 12
    أخرىdried under vacuum

الإجراء التجريبي

A mixture of 4-fluoro-2-(trifluoromethyl)benzonitrile (5.67 g, 30 mmoles), 5,5-dimethyl-hydantoin (7.68 g, 60 mmoles), K2CO3 (8.28 g, 60 mmoles) in DMF (45 ml) is distributed in equal parts into three tubes to be placed in a microwave oven. Under magnetic stirring, each tube is irradiated at 140° C. for 20 minutes. The reaction masses are then combined, poured into water (200 ml) and extracted with AcOEt (2×75 ml). The organic phases are combined, washed with salt water, dried over Na2SO4 and filtered. The filtrate is concentrated under reduced pressure and the residue crystallizeds from Et2O (25 ml). After recrystallization from EtOH (75 ml), the powder is filtered and dried under vacuum. The expected compound is obtained in the form of a white solid with a yield of 46% (4.1 g). Melting point: 212-213° C.

المصدر