反应详情

18 g (46.5 mM) of 8α-benzyloxycarbonylamino-6-cyanoergoline obtained from step (b) in 100 ml acetic acid are added to a suspension of 40 g zinc in 100 ml acetic acid. 40 ml water are added and the mixture is heated at 100° for 10 hours. To work up, the mixture is filtered through a filtering aid such as Hyflo and concentrated in a rotary evaporator. The residue is partitioned between potassium bicarbonate aqueous solution and methylene chloride/isopropanol (b 9:1). The organic phase is dried over sodium sulphate, filtered and concentrated to give the heading compound in crude form.

1. temperaturethe mixture is heated at 100° for 10 hours
2. filtrationthe mixture is filtered through a filtering aid such as Hyflo
3. concentrationconcentrated in a rotary evaporator
4. customThe residue is partitioned between potassium bicarbonate aqueous solution and methylene chloride/isopropanol (b 9:1)
5. dry with materialThe organic phase is dried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated
8. customto give the heading compound in crude form