反应详情

温度

120 °C

X-Phos (35 mg, 0.0739 mmol) and Pd2(dba)3 (45 mg, 0.0492 mmol) were added to a previously degassed solution of 3,4-dihydro-2H-benzo[4,5]thieno[3,2-c]pyridin-1-one (I-9d: 100 mg, 0.4919 mmol), K3PO4 (313 mg, 1.4759 mmol) and 1,4-dioxane (5 mL) in a sealed tube. This was followed by the addition of 3-bromo-4-(trifluoromethyl)pyridine (134 mg, 0.5903 mmol) and the resulting reaction mass was heated at 120° C. for 48 hours. The reaction was monitored by TLC (50% ethyl acetate in hexane). The reaction mass was partitioned between water and ethylacetate. The organic layer was washed with water, brine solution, dried over Na2SO4 and concentrated to afford the crude product. Purification by column chromatography on silica gel (30% ethyl acetate in hexane), followed by preparative HPLC afforded 14 mg of the product (8.18% yield).

1. customthe resulting reaction mass
2. customThe reaction mass was partitioned between water and ethylacetate
3. washThe organic layer was washed with water, brine solution
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto afford the crude product
7. customPurification by column chromatography on silica gel (30% ethyl acetate in hexane)