反应详情

温度

120 °C

To 1.50 g (7.25 mmol) of 4-bromo-5-fluorobenzene-1,2-diol in 25 ml DMF are added 5.90 g (18.1 mmol) Cs2CO3 and 0.89 ml (8.70 mmol) 1,3-dibromopropane. The reaction mixture is stirred at 120° C. over night. The solvent is removed in vacuo and to the residue is added water. After extracting with EtOAc the org. phases are combined, washed with sat. aq. NaCl solution and dried over MgSO4. The solvent is removed in vacuo and the resulting residue is purified by column chromatography (silica gel, PE/EtOAc 9/1→7/3).

1. customThe solvent is removed in vacuo and to the residue
2. additionis added water
3. extractionAfter extracting with EtOAc the org
4. washwashed with sat. aq. NaCl solution
5. dry with materialdried over MgSO4
6. customThe solvent is removed in vacuo
7. customthe resulting residue is purified by column chromatography (silica gel, PE/EtOAc 9/1→7/3)