反応 #64129

反応方程式

aluminum chloride

dichloromethyl methyl ether

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

tartaric acid

ammonia

→

2-Bromo-8alpha-(3,3-diethylureido)-6-methyl-ergoline-13-carbaldehyde

溶媒

dichloromethane

water

反応条件

後処理

1. 1
   抽出It is extracted with dichloromethane
2. 2
   乾燥the organic phases are dried with sodium sulfate
3. 3
   workup.DISTILLATIONthe solvent is distilled off
4. 4
   その他The residue is chromatographed on silica gel with dichloromethane/methanol
5. 5
   その他406 mg (45% of theory) is isolated

実験手順

838 mg of 3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea (2 mmol) is dissolved in 100 ml of dichloromethane, 1.2 g of anhydrous aluminum chloride (9 mmol) and 1.8 ml of dichloromethyl methyl ether (20 mmol) are added and stirred for 15 minutes at room temperature. The reaction mixture is mixed with ice and, after 15 minutes, with a solution of 1.5 g of tartaric acid in 50 ml of water and made alkaline with 5 ml of conc. ammonia solution. It is extracted with dichloromethane, the organic phases are dried with sodium sulfate and the solvent is distilled off. The residue is chromatographed on silica gel with dichloromethane/methanol, 406 mg (45% of theory) is isolated.

出典