1,4-diazepan-6-ylmethanol

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

実験手順: 2.26 g (7.3 mmol) of (1,4-dibenzyl-[1,4]-diazepan-6-yl)-methanol are dissolved in 150 ml of methanol and hydrogenated at room temperature and normal pressure in the presence of 0.5 g of 10% palladium on activated charcoal. [1,4]-Diazepan-6-yl-methanol is obtained in the form of a light yellow oil by filtration and concentration of the filtrate.

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

実験手順: 2.26 g (7.3 mmol) of (1,4-dibenzyl-[1,4]-diazepan-6-yl)-methanol are dissolved in 150 ml of methanol and hydrogenated at room temperature and normal pressure in the presence of 0.5 g of 10% palladium on activated charcoal. [1,4]-Diazepan-6-yl-methanol is obtained in the form of a light yellow oil by filtration and concentration of the filtrate.

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

実験手順: 2.26 g (7.3 mmol) of (1,4-dibenzyl-[1,4]-diazepan-6-yl)-methanol are dissolved in 150 ml of methanol and hydrogenated at room temperature and normal pressure in the presence of 0.5 g of 10% palladium on activated charcoal. [1,4]-Diazepan-6-yl-methanol is obtained in the form of a light yellow oil by filtration and concentration of the filtrate.

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

実験手順: ([1,4]Diazepan-6-yl)methanol (1C) including potassium carbonate salts (ca 1 mmol) was suspended in dry DMF (200 ml) and 7-benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-purine-2,6-dione (199.9 mg, 0.656 mmol) and potassium carbonate (453 mg, 3.28 mmol) were added. The reaction mixture was stirred at room temperature for 24 hours, heated to 60° C. for 3 hours, heated to 95° C. for 5 hours and heated to 120° C. for 2 hours. The suspension was allowed to cool to room temperature and white salts were filtered off. The filtrate was evaporated and purified by chromatography on silica, using 5% methanol in dichloromethane as the eluent. Fractions containing the product were evaporated and purified by preparative HPLC (method A2; Rt=2.52 min.) to afford 8 mg of the title compound as an yellow oil in 1% yield. heated to 60° C. for 3 hours heated to 95° C. for 5 hours heated to 120° C. for 2 hours to cool to room temperature white salts were filtered off The filtrate was evaporated purified by chromatography on silica Fractions containing the product were evaporated purified by preparative HPLC (method A2; Rt=2.52 min.)

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

実験手順: 2.26 g (7.3 mmol) of (1,4-dibenzyl-[1,4]-diazepan-6-yl)-methanol are dissolved in 150 ml of methanol and hydrogenated at room temperature and normal pressure in the presence of 0.5 g of 10% palladium on activated charcoal. [1,4]-Diazepan-6-yl-methanol is obtained in the form of a light yellow oil by filtration and concentration of the filtrate.