反应详情

温度

80 °C

A mixture of the product of Example 22, Step 3, benzyl (1-(5-bromopyridin-2-yl)ethyl)carbamate, 2.0M sodium carbonate in water (3.1 mL, 6.2 mmol) in dioxane is degassed with nitrogen. 1,1′-bis(diphenylphosphino)ferrocene dichloropalladium(ii) complex with dichloromethane (169 mg, 0.21 mmol) is added and the mixture heated to 80° C. overnight. After cooling to room temperature the reaction mixture is diluted with water (25 mL) and extracted with ethylacetate. The organic phase is separated, dried over MgSO4, and concentrated under reduced pressure. The crude material is purified using silica chromatography eluting from 25% ethylacetate/heptane to 35% ethylacetate/heptane to give the title product (1.00 g): m/z: 541.22.

1. customis degassed with nitrogen
2. temperatureAfter cooling to room temperature the reaction mixture
3. extractionextracted with ethylacetate
4. customThe organic phase is separated
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe crude material is purified
8. washeluting from 25% ethylacetate/heptane to 35% ethylacetate/heptane