反应详情

温度

100 °C

A solution of tBuOK in THF (20% wt, 561.0 uL, 1.0 mmol) was added to a mixture of 2-fluoronicotinic acid (70.6 mg, 0.50 mmol) and tetraethyleneglycol monomethyl ether (105.5 μL, 0.50 mmol) in THF (2.0 mL) at ambient temperature under N2. The mixture was heated at 100° C. for 3 h. The reaction mixture was diluted with EtOAc. The organic phase was acidified with 1 N HCl solution, washed with saturated NaCl solution, then dried over Na2SO4. Filtration and concentration in vacuo provided compound D as light yellow liquid (148.1 mg, 90%) for next step without further purification. ESMS: 330.0 [M+H]+, 352.0 [M+Na]+, 368.0 [M+K]+.

1. washwashed with saturated NaCl solution
2. dry with materialdried over Na2SO4
3. filtrationFiltration and concentration in vacuo