反应详情

温度

0 °C

To a solution of N-(2,2,-Dimethyl-2,3-dihydrobenzofuran-7-ylmethyl)-N-(2-phenoxy phenyl)amine (0.20 g, 0.58 mmol) dissolved in DCM (2 mL) was added TEA (0.24 g, 2.32 mmol, 0.32 mL). The reaction was cooled to 0° C. and fluoroacetyl chloride (0.11 g, 1.16 mmol, 0.08 mL) was added. The mixture was stirred at room temperature for 1 h. The solvents were removed in vacuo, the residue quenched with water (10 mL), extracted with DCM (2×20 mL), dried over MgSO4, filtered and solvents removed in vacuo. The crude material was purified by silica gel chromatography eluting with DCM (A) and MeOH (B) (1% B, 80 g, 2 CV, 60 mL/min) to afford 170 mg (72%) of N-(2,2,-Dimethyl-2,3-dihydrobenzofuran-7-ylmethyl)-2-Fluoro-N-(2-phenoxy phenyl)acetamide as a pale yellow oil.

1. customThe solvents were removed in vacuo
2. customthe residue quenched with water (10 mL)
3. extractionextracted with DCM (2×20 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customsolvents removed in vacuo
7. customThe crude material was purified by silica gel chromatography
8. washeluting with DCM (A) and MeOH (B) (1% B, 80 g, 2 CV, 60 mL/min)