تفاعل #166295

معادلة التفاعل

5-Bromo-2,4-dichloro-pyrimidine

cyclohexyl-phenyl-amine

→

compound 37

المردود 24.0%

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

المردود 24.0%

المذيبات

ethyl acetate

N-methylpyrrolidone

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction was cooled to room temperature
2. 2
   غسيلwashed with water and brine
3. 3
   أخرىThe organic phase was dried
4. 4
   تركيزconcentrated
5. 5
   أخرىPurification by flash chromatography (ethyl acetate/hexane)

الإجراء التجريبي

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).

المصدر