反应详情

Trifluoroacetic acid (8 mL) was added to a solution of [1-(4-hydroxy-cyclohexyl)-1-phenyl-ethyl]-carbamic acid tert-butyl ester (29) in dichloromethane (75 mL) from the previous stage. After stirring for 4 hours the reaction mixture was worked up by adding 2M aqueous hydrochloric acid (39 mL), followed by evaporation. Freeze drying overnight gave a pale brown semi-solid residue. This was treated with a mixture of water and acetonitrile. After freeze drying again 1.24 g of crude product as the hydrochloride was obtained which was used in the next stage without further purification. Rt=0.58 min (Method 5). Detected mass: 185.15 (M—NH3—H2O+H+).

1. customfollowed by evaporation
2. customFreeze drying overnight
3. customgave a pale brown semi-solid residue
4. dry with materialAfter freeze drying again 1.24 g of crude product as the hydrochloride
5. customwas obtained which
6. customwas used in the next stage without further purification