Reacción #63233

Ecuación de reacción

water

8α-benzyloxycarbonylamino-6-cyanoergoline

→

8α-benzyloxycarbonylaminoergoline

Disolventes

acetic acid

acetic acid

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturathe mixture is heated at 100° for 10 hours
2. 2
   Filtraciónthe mixture is filtered through a filtering aid such as Hyflo
3. 3
   Concentraciónconcentrated in a rotary evaporator
4. 4
   OtroThe residue is partitioned between potassium bicarbonate aqueous solution and methylene chloride/isopropanol (b 9:1)
5. 5
   SecadoThe organic phase is dried over sodium sulphate
6. 6
   Filtraciónfiltered
7. 7
   Concentraciónconcentrated
8. 8
   Otroto give the heading compound in crude form

Procedimiento

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.

Fuente