反应详情

温度

0 °C

To a cooled (0° C.) stirring suspension of aluminum chloride (10.89 g, 82 mmol) in DCE (700 ml) is added 2-bromopropionyl bromide (8.66 ml, 82 mmol) followed by 3-chloroanisol (10 ml, 82 mmol) dropwise (rapidly) maintaining the temperature below 5° C. The reaction mixture is stirred at 0° C. for 10 min and RT for 3 hours. The mixture is poured into ice/water (1000 ml) containing 90 ml of 5M HCl. The organic phase is separated and the aqueous portion is washed with DCM (500 ml). The organic extracts are combined, washed with brine, dried (MgSO4) and concentrated in vacuo. Purification of the crude product by chromatography on silica eluting with 2.5% incraesing to 5% TBME/Hex increasing up to 5% affords the title product. MS: m/z 278.9 [M+H]+

1. temperaturemaintaining the temperature below 5° C
2. stirringThe reaction mixture is stirred at 0° C. for 10 min and RT for 3 hours
3. customThe organic phase is separated
4. washthe aqueous portion is washed with DCM (500 ml)
5. washwashed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo
8. customPurification of the crude product by chromatography on silica eluting with 2.5%
9. temperatureincreasing up to 5%