Reaktion #64136

Reaktionsgleichung

dichloromethane

3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

trichloroisocyanuric acid

ammonia

→

3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

Lösungsmittel

trifluoroacetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONice is added
2. 2
   SonstigeThe organic phases are dried
3. 3
   Einengenconcentrated by evaporation
4. 4
   Sonstigethe residue is chromatographed
5. 5
   Sonstigethe product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory)

Vorschrift

2.1 g of 3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea (5 mmol) and 388 mg of trichloroisocyanuric acid (1.67 mmol) are dissolved in 100 ml of trifluoroacetic acid at room temperature. After 15 minutes, ice is added, it is made alkaline with conc. ammonia and shaken out with dichloromethane. The organic phases are dried and concentrated by evaporation, the residue is chromatographed and the product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory).

Quelle