Reaktion #63494

Reaktionsgleichung

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

Ausbeute 97.9%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled in an ice bath
2. 2
   Extraktionextracted
3. 3
   SonstigeAfter drying
4. 4
   Sonstigeevaporation of the organic phase

Vorschrift

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).

Quelle