反応 #555753

反応方程式

water

4-fluoro-2-(trifluoromethyl)benzonitrile

5,5-dimethyl-hydantoin

K2CO3

→

expected compound

収率 46.0%

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

収率 46.0%

溶媒

DMF

反応条件

後処理

1. 1
   その他to be placed in a microwave oven
2. 2
   その他Under magnetic stirring, each tube is irradiated at 140° C. for 20 minutes
3. 3
   その他The reaction masses
4. 4
   抽出extracted with AcOEt (2×75 ml)
5. 5
   洗浄washed with salt water
6. 6
   乾燥dried over Na2SO4
7. 7
   ろ過filtered
8. 8
   濃縮The filtrate is concentrated under reduced pressure
9. 9
   その他the residue crystallizeds from Et2O (25 ml)
10. 10
    その他After recrystallization from EtOH (75 ml)
11. 11
    ろ過the powder is filtered
12. 12
    その他dried under vacuum

実験手順

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.

出典