Réaction #63494

Équation de réaction

ammonia

3-(2,3β-dihydro-6-methyl-12-nitro-8α-ergolinyl)-1,1-diethylurea

sodium borohydride

hydrochloric acid

→

3-(12-amino-2,3-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea

Rendement 97.9%

Solvants

methanol

Conditions de réaction

Traitement

1. 1
   Températurecooled in an ice bath
2. 2
   Extractionextracted
3. 3
   AutreAfter drying
4. 4
   Autreevaporation of the organic phase

Mode opératoire

One millimole of 3-(2,3β-dihydro-6-methyl-12-nitro-8α-ergolinyl)-1,1-diethylurea is dissolved in 25 ml of methanol, cooled in an ice bath, and 2 mmol of nickel chloride (with 6H2O) and thereafter 5 mmol of sodium borohydride are added thereto in 4-5 portions. Under ice cooling, the mixture is acidified with 2N hydrochloric acid, combined with dilute ammonia solution, and extracted by shaking. After drying and evaporation of the organic phase, 350 mg of 3-(12-amino-2,3-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea is obtained. [α]D =-31° (0.5% methanol) as the tartaric acid salt (1:1).

Source