반응 #164882

반응 방정식

3-Iodo-4-methylaniline

triethylamine

3-fluoro-5-(trifluoromethyl)benzoyl chloride

→

3-Fluoro-N-(3-iodo-4-methylphenyl)-5-(trifluoromethyl)benzamide

용매

DCM

반응 조건

후처리

1. 1
   추출The reaction was extracted with ethyl acetate
2. 2
   세척the organic extracts were washed with water sat. Na2CO3, saturated NaCl
3. 3
   건조dried (MgSO4)
4. 4
   농축concentrated in vacuo
5. 5
   기타The reaction product was used in the next reaction without purification

실험 절차

3-Iodo-4-methylaniline (2.42 g, 10.4 mmol) was dissolved in DCM (20.00 mL) and triethylamine (TEA) (1.70 mL, 12.2 mmol) was added and the resulting mixture was cooled to 0° C. To the mixture was added dropwise 3-fluoro-5-(trifluoromethyl)benzoyl chloride (1.60 mL, 10.5 mmol) and the resulting mixture was stirred at 0° C. for 45 minutes and at 25° C. for 16 hours. The reaction was extracted with ethyl acetate and the organic extracts were washed with water sat. Na2CO3, saturated NaCl, dried (MgSO4) and concentrated in vacuo. The reaction product was used in the next reaction without purification. 1H NMR (CDCl3): δ □ 8.98 (d, 1H), 7.78 (s, 1H), 7.72 (m, 2H), 7.55 (m, 2H), 7.23 (d, 1H), 2.42 (s, 3H). MS (EI) m/z=424 (M+H).

출처