4-(2-羟乙基)哌嗪-1-碳硫酰胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5 g of 4-(2-hydroxyethyl)-1-piperazinyl-thiocarboxamide are added to a solution of 3.6 g of bromopinacoline in 70 cc of ethanol, and the reaction mixture is subsequently heated to the boil at reflux for 2 hours. The mixture is then concentrated by evaporation in a vacuum. The residue is dissolved in a small amount of water and is divided between chloroform and a concentrated aqueous sodium hydroxide solution. The chloroform phase is washed with water, dried over sodium sulphate and concentrated by evaporation in a vacuum. Hydrochloric acid in ethanol is added to the resulting oil and the solution is concentrated by evaporation. After recrystallizing the residue from a small amount of ethanol/diethyl ether, 2-[4-(2-hydroxyethyl)-1-piperazinyl]-4-tert.butyl-thiazole dihydrochloride, having a M.P. of 133°-142°, is obtained. The free base is obtained is known manner from the dihydrochloride by treatment with an aqueous sodium hydroxide solution. the reaction mixture is subsequently heated to the boil at reflux for 2 hours The mixture is then concentrated by evaporation in a vacuum The residue is dissolved in a small amount of water The chloroform phase is washed with water dried over sodium sulphate concentrated by evaporation in a vacuum Hydrochloric acid in ethanol is added to the resulting oil the solution is concentrated by evaporation After recrystallizing the residue from a small amount of ethanol/diethyl ether, 2-[4-(2-hydroxyethyl)-1-piperazinyl]-4-tert.butyl-thiazole dihydrochloride is obtained The free base is obtained

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5 g of 4-(2-hydroxyethyl)-1-piperazinyl-thiocarboxamide are added to a solution of 3.6 g of bromopinacoline in 70 cc of ethanol, and the reaction mixture is subsequently heated to the boil at reflux for 2 hours. The mixture is then concentrated by evaporation in a vacuum. The residue is dissolved in a small amount of water and is divided between chloroform and a concentrated aqueous sodium hydroxide solution. The chloroform phase is washed with water, dried over sodium sulphate and concentrated by evaporation in a vacuum. Hydrochloric acid in ethanol is added to the resulting oil and the solution is concentrated by evaporation. After recrystallizing the residue from a small amount of ethanol/diethyl ether, 2-[4-(2-hydroxyethyl)-1-piperazinyl]-4-tert.butyl-thiazole dihydrochloride, having a M.P. of 133°-142°, is obtained. The free base is obtained is known manner from the dihydrochloride by treatment with an aqueous sodium hydroxide solution. the reaction mixture is subsequently heated to the boil at reflux for 2 hours The mixture is then concentrated by evaporation in a vacuum The residue is dissolved in a small amount of water The chloroform phase is washed with water dried over sodium sulphate concentrated by evaporation in a vacuum Hydrochloric acid in ethanol is added to the resulting oil the solution is concentrated by evaporation After recrystallizing the residue from a small amount of ethanol/diethyl ether, 2-[4-(2-hydroxyethyl)-1-piperazinyl]-4-tert.butyl-thiazole dihydrochloride is obtained The free base is obtained

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5 g of 4-(2-hydroxyethyl)-1-piperazinyl-thiocarboxamide are added to a solution of 3.6 g of bromopinacoline in 70 cc of ethanol, and the reaction mixture is subsequently heated to the boil at reflux for 2 hours. The mixture is then concentrated by evaporation in a vacuum. The residue is dissolved in a small amount of water and is divided between chloroform and a concentrated aqueous sodium hydroxide solution. The chloroform phase is washed with water, dried over sodium sulphate and concentrated by evaporation in a vacuum. Hydrochloric acid in ethanol is added to the resulting oil and the solution is concentrated by evaporation. After recrystallizing the residue from a small amount of ethanol/diethyl ether, 2-[4-(2-hydroxyethyl)-1-piperazinyl]-4-tert.butyl-thiazole dihydrochloride, having a M.P. of 133°-142°, is obtained. The free base is obtained is known manner from the dihydrochloride by treatment with an aqueous sodium hydroxide solution. the reaction mixture is subsequently heated to the boil at reflux for 2 hours The mixture is then concentrated by evaporation in a vacuum The residue is dissolved in a small amount of water The chloroform phase is washed with water dried over sodium sulphate concentrated by evaporation in a vacuum Hydrochloric acid in ethanol is added to the resulting oil the solution is concentrated by evaporation After recrystallizing the residue from a small amount of ethanol/diethyl ether, 2-[4-(2-hydroxyethyl)-1-piperazinyl]-4-tert.butyl-thiazole dihydrochloride is obtained The free base is obtained