1-苄基-2,2-二甲基哌嗪

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 1-benzyl-2,2-dimethylpiperazine (1.2 g, 5.87 mmol) in 1,4-dioxane (50 ml) at 25° C. was added 1-bromo-4-fluorobenzene (1.233 g, 7.05 mmol), 2,2′-Bis(diphenylphosphino)-1,1′-binaphthyl (BINAP) (0.366 g, 0.587 mmol), sodium tert-butoxide (1.129 g, 11.75 mmol), and tris(dibenzyllideneacetone)dipalladium (0) [Pd2(dba)3] (0.269 g, 0.294 mmol). The reaction mixture was purged with nitrogen for 10 min in sealed tube and then heated at 100° C. for 5 h. The progress of reaction was monitored by TLC. The reaction mixture was cooled to 25° C., filtered through celite, washed with ethyl acetate (2×50 ml). The combined filtrate was concentrated under reduced pressure to obtain a crude product. The crude product was purified over silica gel (100-200 mesh) by flash chromatography using 10% ethyl acetate in hexane as eluent to obtain the title compound (1.1 g, 62.8%) The reaction mixture was purged with nitrogen for 10 min in sealed tube The progress of reaction The reaction mixture was cooled to 25° C. filtered through celite washed with ethyl acetate (2×50 ml) The combined filtrate was concentrated under reduced pressure to obtain a crude product The crude product was purified over silica gel (100-200 mesh) by flash chromatography

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of lithiulalluminium hydride (1.078 g, 28.4 mmol) in tetrahydrofuran (200 ml) at 0-20° C. was added 4-benzyl-3,3-dimethylpiperazin-2-one (6.2 g, 28.4 mmol in 100 ml tetrahydrofuran) over 1 h. The reaction mixture was warmed to 25° C. over 15 minutes followed by reflux for 6 h. The progress of reaction was monitored by TLC. After completion of reaction, the reaction mixture was cooled to 0-10° C. and 10% sodium hydroxide (50 ml) was added slowly over 1 h. and then allowed to stir for 20 hr at 25° C. The reaction mass was passed through celite and washed with tetrahydrofuran (500 ml). The combined filtrate was concentrated under reduced pressure. Water (100 ml) was added and the aq. phase was extracted with ethyl acetate (3×100 ml). The combined organic layer was washed with brine (50 ml) and dried over sodium sulphate, and concentrated under reduced pressure till dryness. The resulting crude product (5.2 g) was carried over to the next step without purification. by reflux for 6 h The progress of reaction After completion of reaction the reaction mixture was cooled to 0-10° C. washed with tetrahydrofuran (500 ml) The combined filtrate was concentrated under reduced pressure Water (100 ml) was added the aq. phase was extracted with ethyl acetate (3×100 ml) The combined organic layer was washed with brine (50 ml) dried over sodium sulphate concentrated under reduced pressure till dryness The resulting crude product (5.2 g) was carried over to the next step without purification