반응 #657799

반응 방정식

2-Acetylcyclohexanone

4-Bromo-2-fluoro-N-methylbenzamide

K2CO3

DMF

citric acid

→

2-(4-(methylcarbamoyl)-3-fluorophenylamino)-2-methylpropanoic acid

용매

water

triethylamine

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate (50 mL, 2 times)
2. 2
   건조The organic layer was dried over Na2SO4
3. 3
   농축concentrated

실험 절차

4-Bromo-2-fluoro-N-methylbenzamide (155 mg, 0.66 mmol), isoaminobutyric acid (103 mg, 1.0 mmol), CuI (3 mg, 0.015 mmol), triethylamine (0.1 mL, catalytic amount) and K2CO3 (353 mg, 2.5 mmol) were dissolved in DMF (4 mL) and water (1 mL) stirred at RT for 5 min. 2-Acetylcyclohexanone (100 mg, 0.7 mmol) was added and the mixture heated at 100° C. for 18 h. The reaction mixture was acidified with 1 M citric acid (to pH 4) and extracted with ethyl acetate (50 mL, 2 times). The organic layer was dried over Na2SO4 and concentrated to obtain 200 mg of 2-(4-(methylcarbamoyl)-3-fluorophenylamino)-2-methylpropanoic acid.

출처