反应详情

温度

5 °C

More specifically, adamantane-1-carboxylic acid (1) (45 g, 0.25 mol) was added to mixture of AlCl3 (45 g, 0.34 mol) and Br2 (450 g) at 0° C. and stirred at 0-10° C. for 48 hrs, kept 5 hrs at about 20° C., poured on to 500 g crushed ice, diluted with 300 ml CHCl3 and decolorized with solid Na2S2O5. The aqueous phase was extracted with Et2O (50 ml×2). The combined organic solution was washed with H2O and extracted with 10% NaOH. The alkaline extraction was acidified with 2N H2SO4 and provided 49 g (yield=75.7%) of 3-bromo-adamantane-1-carboxylic acid (2).

1. waitkept 5 hrs at about 20° C.
2. additionpoured on to 500 g
3. customcrushed ice
4. extractionThe aqueous phase was extracted with Et2O (50 ml×2)
5. washThe combined organic solution was washed with H2O
6. extractionextracted with 10% NaOH
7. extractionThe alkaline extraction