反应详情

To a solution of the compound obtained in Step E (7.68 mmoles) in acetic acid (15 ml) there are added TFA (7 ml) and Pd/C 10% (400 mg). The reaction mixture is stirred at 50° C. under 4 bars of hydrogen overnight. The catalyst is filtered off on a bed of Celite and is then washed with acetic acid (20 ml). The filtrate is evaporated to dryness and the residual acetic acid is removed by azeotropic distillation with toluene. The solid obtained is recrystallised from a mixture of EtOH/ethyl ether to yield the title product after drying in vacuo.

1. filtrationThe catalyst is filtered off on a bed of Celite
2. washis then washed with acetic acid (20 ml)
3. customThe filtrate is evaporated to dryness
4. customthe residual acetic acid is removed by azeotropic distillation with toluene
5. customThe solid obtained
6. customis recrystallised from a mixture of EtOH/ethyl ether