1-cyclopropylsulfonylpiperazine;hydrochloride

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 14.37 g of tert-butyl ester of 4-cyclopropanesulfonyl-piperazine-1-carboxylic acid is put in a 2-liter three-necked flask, under nitrogen atmosphere. 412 ml of dichloromethane is added. The reaction mixture is cooled in an ice bath and 4M hydrochloric acid in solution in dioxane is added dropwise. The reaction mixture is allowed to return gradually to room temperature. The reaction mixture is stirred for 2.5 h, then evaporated and concentrated. The residue is taken up in a small amount of ethyl ether, triturated and then filtered and dried. 10.25 g of 1-cyclopropanesulfonyl-piperazine hydrochloride is obtained in the form of a white powder. The reaction mixture is cooled in an ice bath to return gradually to room temperature evaporated concentrated triturated filtered dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 14.37 g of tert-butyl ester of 4-cyclopropanesulfonyl-piperazine-1-carboxylic acid is put in a 2-liter three-necked flask, under nitrogen atmosphere. 412 ml of dichloromethane is added. The reaction mixture is cooled in an ice bath and 4M hydrochloric acid in solution in dioxane is added dropwise. The reaction mixture is allowed to return gradually to room temperature. The reaction mixture is stirred for 2.5 h, then evaporated and concentrated. The residue is taken up in a small amount of ethyl ether, triturated and then filtered and dried. 10.25 g of 1-cyclopropanesulfonyl-piperazine hydrochloride is obtained in the form of a white powder. The reaction mixture is cooled in an ice bath to return gradually to room temperature evaporated concentrated triturated filtered dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 14.37 g of tert-butyl ester of 4-cyclopropanesulfonyl-piperazine-1-carboxylic acid is put in a 2-liter three-necked flask, under nitrogen atmosphere. 412 ml of dichloromethane is added. The reaction mixture is cooled in an ice bath and 4M hydrochloric acid in solution in dioxane is added dropwise. The reaction mixture is allowed to return gradually to room temperature. The reaction mixture is stirred for 2.5 h, then evaporated and concentrated. The residue is taken up in a small amount of ethyl ether, triturated and then filtered and dried. 10.25 g of 1-cyclopropanesulfonyl-piperazine hydrochloride is obtained in the form of a white powder. The reaction mixture is cooled in an ice bath to return gradually to room temperature evaporated concentrated triturated filtered dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidine-6-carbaldehyde was treated with 1-cyclopropanesulfonyl-piperazine hydrochloride using General Procedure C (reductive amination) to yield 2-chloro-6-(4-cyclopropanesulfonyl-piperazin-1-ylmethyl)-4-morpholin-4-yl-thieno[3,2-d]pyrimidine.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidine-6-carbaldehyde was treated with 1-cyclopropanesulfonyl-piperazine hydrochloride using General Procedure C (reductive amination) to yield 2-chloro-6-(4-cyclopropanesulfonyl-piperazin-1-ylmethyl)-4-morpholin-4-yl-thieno[3,2-d]pyrimidine.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To N—BOC-piperazine (1.3 g) in dry DCM (10 ml) was added triethylamine (1.2 mL) and cyclopropanesulphonyl chloride (1.04 g) and the reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was then diluted with DCM, washed with water, dried (MgSO4) and reduced in vacuo. The residue was dissolved in methanol (10 mL) and 4M HCL in dioxane was added (20 mL). After stirring overnight the solvent was reduced in vacuo to yield 1-cyclopropanesulfonyl-piperazine hydrochloride. washed with water dried (MgSO4) The residue was dissolved in methanol (10 mL) 4M HCL in dioxane was added (20 mL) After stirring overnight the solvent