تفاعل #63494

معادلة التفاعل

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

المردود 97.9%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled in an ice bath
2. 2
   استخلاصextracted
3. 3
   أخرىAfter drying
4. 4
   أخرىevaporation of the organic phase

الإجراء التجريبي

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).

المصدر