反应详情

温度

80 °C

To a solution of the product of Step 3, Example 22 (1000 mg, 2.4 mmol) in toluene/ethanol (30:20 mL) is added commercially available tert-butyl (5-bromopyridin-2-yl)methylcarbamate (695 mg, 2.42 mmol), sodium bicarbonate (5 mL of a saturated solution) and Pd(dppf)2Cl2 (90 mg, 0.12 mmol). The reaction mixture is heated to 80° C. while stirring under nitrogen for 4 hours. The reaction mixture is cooled and diluted with water. Contents are extracted with ethylacetate (2×75 mL) and the combined organic phase is dried (Na2SO4) and concentrated under vacuum. Crude material is chromatographed (80 g Redi-Sep column) eluting from 100% hexanes to 90:10 ethylacetate:hexanes to afford the title compound (912 mg): m/z (CI) M+H 494.

1. temperatureThe reaction mixture is cooled
2. extractionContents are extracted with ethylacetate (2×75 mL)
3. dry with materialthe combined organic phase is dried (Na2SO4)
4. concentrationconcentrated under vacuum
5. customCrude material is chromatographed (80 g Redi-Sep column)
6. washeluting from 100% hexanes to 90:10 ethylacetate