反应详情

温度

0 °C

A solution consisting of 3,5-dimethoxy fluorobenzene 26 (5.0 g, 32 mmol) and chloroacetyl chloride (4.3 g, 38 mmol) in dichloroethane (100 mL) was cooled to 0° C. and treated with AlCl3 (5.1 g, 38 mmol). The reaction was allowed to rt and stirred for 1 h and then washed with 2N HCl aq, brine, dried over MgSO4, filtered, concentrated and chromatographed on silica gel (1:9 EtOAc/hexanes to 2:8 EtOAc/hexanes) to yiled th product 27 (1.2 g) as a white solid: Mp 93-96° C.

1. customwas allowed to rt
2. washwashed with 2N HCl aq, brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customchromatographed on silica gel (1:9 EtOAc/hexanes to 2:8 EtOAc/hexanes) to yiled th product 27 (1.2 g) as a white solid