반응 #166295

반응 방정식

5-Bromo-2,4-dichloro-pyrimidine

cyclohexyl-phenyl-amine

→

compound 37

수율 24.0%

(5-Bromo-2-chloro-pyrimidin-4-yl)-cyclohexyl-phenyl-amine

수율 24.0%

용매

ethyl acetate

N-methylpyrrolidone

반응 조건

후처리

1. 1
   온도The reaction was cooled to room temperature
2. 2
   세척washed with water and brine
3. 3
   기타The organic phase was dried
4. 4
   농축concentrated
5. 5
   기타Purification by flash chromatography (ethyl acetate/hexane)

실험 절차

5-Bromo-2,4-dichloro-pyrimidine (2.17 ml, 17.14 mmol) and cyclohexyl-phenyl-amine (2.0 g, 11.43 mmol) were dissolved in N-methylpyrrolidone (NMP) (25 ml), and this reaction was heated to 120° C. for 24 hours. The reaction was cooled to room temperature and diluted with ethyl acetate, washed with water and brine. The organic phase was dried using sodium sulfate and concentrated. Purification by flash chromatography (ethyl acetate/hexane) gave compound 37 as a yellow solid (855 mg, 24%). 1H NMR (500 MHz, DMSO-d6) δ ppm 8.27 (1 H, s), 7.41 (3 H, m), 7.21 (2 H, m), 4.62 (1 H, m), 1.93 (2 H, d, J=10 Hz), 1.75 (2 H, d, J=10 Hz), 1.58 (1 H, d, J=10 Hz), 1.34 (2 H, m), 1.15 (2 H, m), 0.91 (1 H, m).

출처