反应详情

A mixture of ethyl 8-iodo-6-(trifluoromethoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylate prepared as in Example 21a, Step 2 (0.500 g, 1.04 mmole), trimethylboroxine (145 uL, 1.04 mmole), PdCl2(dppf)2.CH2Cl2 (0.084 mg, 0.104 mmole) and Cs2CO3 (1.01 g, 3.11 mmole) in 10% aqueous dioxane (2.5 mL) was heated to 110° C. under a dry N2 atmosphere for 6 h. The mixture was poured into EtOAc (100 mL), washed with brine (2×50 mL), dried over MgSO4, filtered and concentrated in vacuo to give an oily yellow solid. Purification by silica chromatography (9:1 hexanes:EtOAc) gave 0.320 g (83% yield) of the product as a yellow crystalline solid: EIHRMS m/z 370.0650 (M+, C15H2F6O4, 370.0640).

1. washwashed with brine (2×50 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto give an oily yellow solid
6. customPurification by silica chromatography (9:1 hexanes:EtOAc)