反应详情

温度

60 °C

The product from step 2 (3.3 g) is dissolved in POCl3 (25 mL) and the resulting solution stirred at 60° C. for 6 hours. The reaction mixture is cooled, and the volatiles are removed under reduced pressure. Flash chromatography (1-4% ethyl acetate in hexanes) affords 2-chloro-5-(2,4-dimethoxy-phenyl)-3,6-diethyl-pyrazine as a clear oil. MS: 307. H-1 NMR (400 MHz, CDCl3): 1.16 (t, 3H), 1.31 (t, 3H), 2.60 (q, 2H), 3.00 (q, 2H), 3.75 (s, 3H), 3.76 (s, 3H), 6.53 (d, 1H), 6.59 (dd, 1H), 7.19 (d, 1H).

1. temperatureThe reaction mixture is cooled
2. customthe volatiles are removed under reduced pressure