CAS 156094-63-2 2-(broMoMethyl)-6-Methoxypyridine | Products & Prices & Suppliers

1.07 g (6.01 mmol) of N-bromosuccinimide (NBS) and 49.3 mg ( 0.300 mmol) of azobisisobutyronitrile(AIBN) were mixed in 8 mL of carbon tetrachloride (CCl4) under nitrogen atmosphere. Themixture was then heated and 0.73 mL (6.00 mmol) of 2-methoxy-6-methylpyridine was added. Afterrefluxed 8 hours in oil bath, the mixture was cooled to ambient temperature. The crude was thenconcentrated in vacuo, and purified by silica-gel column chromatography [eluent: chroloform /hexane = 1:1 (v/v) ] to give 619 mg (66 percent yield) of 2-bromomethyl-6-methoxypyridine as acolorless liquid. 1H NMR (400 MHz CDCl3) δ 7.55 (dd, J = 8.2 Hz, J = 7.3 Hz, 1H), 7.32 (d, J = 7.3 Hz, 1H), 6.99 (d, J = 8.2 Hz, 1H), 4.56 (s, 2H), 3.94 (s, 3H).1.07 g (6.01 mmol) of N-bromosuccinimide (NBS) and 49.3 mg ( 0.300 mmol) of azobisisobutyronitrile(AIBN) were mixed in 8 mL of carbon tetrachloride (CCl4) under nitrogen atmosphere. Themixture was then heated and 0.73 mL (6.00 mmol) of 2-methoxy-6-methylpyridine was added. Afterrefluxed 8 hours in oil bath, the mixture was cooled to ambient temperature. The crude was thenconcentrated in vacuo, and purified by silica-gel column chromatography [eluent: chroloform /hexane = 1:1 (v/v) ] to give 619 mg (66 percent yield) of 2-bromomethyl-6-methoxypyridine as acolorless liquid. 1H NMR (400 MHz CDCl3) δ 7.55 (dd, J = 8.2 Hz, J = 7.3 Hz, 1H), 7.32 (d, J = 7.3 Hz, 1H), 6.99 (d, J = 8.2 Hz, 1H), 4.56 (s, 2H), 3.94 (s, 3H).A room temperature solution of 4-(6-(piperazin- 1 -yl)pyridin-3 -yl)-6-( 1 H-pyrazol-4- yl)pyrazolo[1, 5-a]pyridine-3-carbonitrile bis(2, 2, 2-trifluoroacetate) (Example 698, Step 1; 6 mg, 0.0162 mmol) in dry DMA (900 tL) was treated sequentially with TEA (22.6 tL, 0.162 mmol) and