1-(2-甲基苯基)哌嗪

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

实验步骤: First, 2-chlorobromoethane (48 g) is added to a solution of 2-methylbenzylpiperazine (12 g) and triethylamine (32 g). The resulting mixture is refluxed for 30 minutes; water is then added and the product is extracted with ether, dried (magnesium sulfate) and concentrated in vacuo to give an oil, which is purified on a silica gel column (methylene chloride: methanol, 9:1). The resulting oil is dissolved in ether and the salt precipitated with ethereal hydrochloric acid to give 9.2 g of 1-(2-chloroethyl)-4-(2-methylbenzyl)piperazine dihydrochloride as colorless crystals. The resulting mixture is refluxed for 30 minutes the product is extracted with ether dried (magnesium sulfate) concentrated in vacuo to give an oil, which is purified on a silica gel column (methylene chloride: methanol, 9:1) The resulting oil is dissolved in ether the salt precipitated with ethereal hydrochloric acid

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

实验步骤: First, 2-chlorobromoethane (48 g) is added to a solution of 2-methylbenzylpiperazine (12 g) and triethylamine (32 g). The resulting mixture is refluxed for 30 minutes; water is then added and the product is extracted with ether, dried (magnesium sulfate) and concentrated in vacuo to give an oil, which is purified on a silica gel column (methylene chloride: methanol, 9:1). The resulting oil is dissolved in ether and the salt precipitated with ethereal hydrochloric acid to give 9.2 g of 1-(2-chloroethyl)-4-(2-methylbenzyl)piperazine dihydrochloride as colorless crystals. The resulting mixture is refluxed for 30 minutes the product is extracted with ether dried (magnesium sulfate) concentrated in vacuo to give an oil, which is purified on a silica gel column (methylene chloride: methanol, 9:1) The resulting oil is dissolved in ether the salt precipitated with ethereal hydrochloric acid

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

实验步骤: First, 2-chlorobromoethane (48 g) is added to a solution of 2-methylbenzylpiperazine (12 g) and triethylamine (32 g). The resulting mixture is refluxed for 30 minutes; water is then added and the product is extracted with ether, dried (magnesium sulfate) and concentrated in vacuo to give an oil, which is purified on a silica gel column (methylene chloride: methanol, 9:1). The resulting oil is dissolved in ether and the salt precipitated with ethereal hydrochloric acid to give 9.2 g of 1-(2-chloroethyl)-4-(2-methylbenzyl)piperazine dihydrochloride as colorless crystals. The resulting mixture is refluxed for 30 minutes the product is extracted with ether dried (magnesium sulfate) concentrated in vacuo to give an oil, which is purified on a silica gel column (methylene chloride: methanol, 9:1) The resulting oil is dissolved in ether the salt precipitated with ethereal hydrochloric acid

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

实验步骤: Analogously to Example 55, 1.5 g of 4-[N-(2-isopropyloxyethyl)-N-chloroacetylamino]benzoyl chloride are reacted with 0.76 g of 2-methylbenzylpiperazine, yielding 1-{4-[N-(2-isopropyloxyethyl)-N-chloroacetylamino]benzoyl}-4-(2-methylbenzyl)piperazine. The hydrochloride thereof melts at 142°-143°.