反应详情

温度

20 °C

A mixture of 2.33 g (10 mmol) (1R,2R)-3-(2-dimethylaminomethyl-cyclohexyl)-phenol, 3.58 g (9 mmol) acetobromo-α-D-glucuronic acid methyl ester and 0.23 g (9.5 mmol) lithium hydroxide in 23 ml dry methanol was first stirred at 20° C. for 30 minutes, a solution of 0.65 g lithium hydroxide in 25 ml water was then added and the mixture was stirred again for 30 minutes. It was extracted with ethyl acetate and the aqueous phase was adjusted to a pH of 3.5 by addition of acetic acid and extracted again with ethyl acetate. The aqueous phase was evaporated in vacuo and the residue was purified by HPLC. 0.85 g (23% of theory) of the title compound was obtained in this manner in the form of a white powder.

1. stirringthe mixture was stirred again for 30 minutes
2. extractionIt was extracted with ethyl acetate
3. additionthe aqueous phase was adjusted to a pH of 3.5 by addition of acetic acid
4. extractionextracted again with ethyl acetate
5. customThe aqueous phase was evaporated in vacuo
6. customthe residue was purified by HPLC