반응 #63487

반응 방정식

ammonia

nitric acid

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

→

3-(2,3-dihydro-6-methyl-13-nitro-8α-ergolinyl)-1,1-diethylurea

수율 71.0%

용매

sulfuric acid

sulfuric acid

반응 조건

후처리

1. 1
   workup.ADDITIONThe reaction solution is then slowly introduced dropwise into ice
2. 2
   추출extracted
3. 3
   workup.STIRRINGby shaking with methylene chloride
4. 4
   세척After washing the organic phase with water
5. 5
   건조drying with magnesium sulfate
6. 6
   기타the nitrated compound is obtained in a 90% crude yield
7. 7
   기타After chromatographic separation and purification

실험 절차

Under ice cooling, 10 mmol of 3-(2,3-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea is dissolved in 100 ml of concentrated sulfuric acid; 7 ml of a solution of 10 ml of 65% nitric acid in 90 ml of concentrated sulfuric acid is added thereto, and the mixture is stirred for 15 minutes in an ice bath. The reaction solution is then slowly introduced dropwise into ice, made alkaline under ice cooling with 32% ammonia solution, and extracted by shaking with methylene chloride. After washing the organic phase with water and drying with magnesium sulfate, the nitrated compound is obtained in a 90% crude yield. After chromatographic separation and purification, respectively, 3-(2,3-dihydro-6-methyl-13-nitro-8α-ergolinyl)-1,1-diethylurea is obtained in a 71% yield.

출처