1-(4-氟苯甲酰基)哌嗪

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: Working as described in Example 3 but replacing 2-(2-chloroethyl)-6,7-dimethoxy-1(2H)-phthalazinone with an equivalent amount of 2-(3-chloropropyl)-6,7-dimethoxy-1(2H)-phthalazinone obtained as described in Example 13, and replacing N-phenylpiperazine with an equivalent amount of 4-(4-fluorobenzoyl)-piperazine, 2-{3-[4-(4-fluorobenzoyl)-piperidin-1-yl]-propyl}-6,7-dimethoxy-1(2H)-phthalazinone hydrochloride is obtained (m.p. 250°-252° C., from ethyl acetate). obtained

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Concentrated hydrochloric acid was added dropwise to a solution of piperazine (0.124 mol) in water (110 ml) to adjust the pH to 2.8. The solution was then heated to 50° C. 4-Fluorobenzoyl chloride (0.124 mol) was added to the warm solution dropwise while maintaining the pH at 2.8 by the concurrent addition of 40% aqueous sodium acetate solution. After complete addition, a solution of potassium carbonate (47 g) in water (50 ml) was added and the mixture cooled in an ice bath. The cold mixture was extracted with chloroform (5×150 ml). The combined extracts were dried (MgSO4) and evaporated in vacuo affording 22.5 g of a white solid (88% yield). Spectral data are consistent with the assigned structure. This material was used without further purification. while maintaining the pH at 2.8 After complete addition the mixture cooled in an ice bath The cold mixture was extracted with chloroform (5×150 ml) The combined extracts were dried (MgSO4) evaporated in vacuo

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

实验步骤: Working as described in Example 3 but replacing 2-(2-chloroethyl)-6,7-dimethoxy-1(2H)-phthalazinone with an equivalent amount of 2-(3-chloropropyl)-6,7-dimethoxy-1(2H)-phthalazinone obtained as described in Example 13, and replacing N-phenylpiperazine with an equivalent amount of 4-(4-fluorobenzoyl)-piperazine, 2-{3-[4-(4-fluorobenzoyl)-piperidin-1-yl]-propyl}-6,7-dimethoxy-1(2H)-phthalazinone hydrochloride is obtained (m.p. 250°-252° C., from ethyl acetate). obtained