反应详情

温度

80 °C

A mixture of 21.3 g of 3-bromophenylglycine in 160 cm3 of 6.5N hydrochloric ethanol is heated with stirring for 24 hours at a temperature in the region of 80° C. The reaction medium is filtered and the filter cake is then washed with twice 30 cm3 of ethanol. The filtrate is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. An oil is obtained, which is basified by addition of aqueous sodium carbonate solution. The mixture is extracted with 3 times 100 cm3 of ethyl acetate. The extracts are combined, washed with twice 100 cm3 of aqueous sodium chloride solution, dried over sodium sulfate, filtered and then concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 4.7 g of ethyl 3-bromophenylglycinate are obtained in the form of a yellow oil. (Rf=0.38 in a 90/5 by volume dichloromethane/methanol mixture, on a Merck 60F254R silica plate).

1. temperatureis heated
2. filtrationThe reaction medium is filtered
3. washthe filter cake is then washed with twice 30 cm3 of ethanol
4. concentrationThe filtrate is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C
5. customAn oil is obtained
6. extractionThe mixture is extracted with 3 times 100 cm3 of ethyl acetate
7. washwashed with twice 100 cm3 of aqueous sodium chloride solution
8. dry with materialdried over sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C