反应详情

温度

150 °C

A solution of ethyl 2-(3,5-dibromopyrazin-2-ylamino)acetate (500 mg, 1.47 mmol), ((trans)-4-methoxycyclohexyl)methanamine (317 mg, 2.21 mmol) and diisopropylethyl amine (0.77 mL, 4.42 mmol) in anhydrous dimethylsulfoxide (8.0 mL) was placed in a microwave vessel (20 mL). The reaction was heated to 150° C. for 1 h. The reaction was poured into water, extracted with ethyl acetate (2×100 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The resulting material was dissolved in acetic acid (30 mL) and placed in a sealed tube. The reaction was heated to 120° C. overnight. The solution was cooled, concentrated under reduced pressure, neutralized with saturated sodium bicarbonate, extracted with ethyl acetate (3×100 mL), dried over sodium sulfate, filtered and adsorbed onto silica gel. Purification by flash chromatography (50% ethyl acetate in hexanes) gave a light orange solid (400 mg, 1.12 mmol, 76% yield). MS (ESI) m/z 355.2 [M+]+, 357.2 {M+2]+.

1. extractionextracted with ethyl acetate (2×100 mL)
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. dissolutionThe resulting material was dissolved in acetic acid (30 mL)
6. customplaced in a sealed tube
7. temperatureThe reaction was heated to 120° C. overnight
8. temperatureThe solution was cooled
9. concentrationconcentrated under reduced pressure
10. extractionextracted with ethyl acetate (3×100 mL)
11. dry with materialdried over sodium sulfate
12. filtrationfiltered
13. customPurification by flash chromatography (50% ethyl acetate in hexanes)