4-methyl-1,4-diazepan-2-one

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A solution of 750 g of N-methyl-N-(2-cyanoethyl)glycine ethyl ester (prepared from methylaminopropionitrile and ethyl chloroacetate) in 1 liter of ethanol is hydrogenated in the presence of 60 g of Raney cobalt in an autoclave at a temperature of from 80° to 90°C and under a pressure of 100 to 120 atms. of hydrogen. The calculated quantity of hydrogen has been absorbed after about 1 hour. The hydrogenated solution is filtered off from the catalyst. The solid residue left after the ethanol has been evaporated is freed from any greases adhering to it by means of a little ethyl acetate, and the white product, which does not show any tendency towards discoloration in air, is fractionated in a high vacuum with 5 g of sodium methoxide. 424 g of 1-N-methyl-hexahydro-1,4-diazepin-3-one melting at 91°C are obtained. The calculated quantity of hydrogen has been absorbed after about 1 hour The hydrogenated solution is filtered off from the catalyst The solid residue left after the ethanol has been evaporated

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A mixture of 4-iodoaniline (70 mg, 0.32 mmol), 4-methyl-2-homopiperazinone (35 mg, 0.27 mmol), K3PO4 (135 mg, 0.64 mmol) and 1,2-trans-diaminocyclohexane (16 uL, 0.13 mmol) in dioxane (4 mL) was degassed with Ar before being charged with CuI (18 mg, 0.095 mmol). The mixture in a sealed tube was heated at 110 C overnight. The mixture was then purified by a silica gel prep-TLC using CH2Cl2/MeOH (95/5) as solvents to give the titled compound (9 mg). MS 220.5 (M+H). was degassed with Ar The mixture in a sealed tube was heated at 110 C overnight The mixture was then purified by a silica gel prep-TLC

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

実験手順: A solution of 750 g of N-methyl-N-(2-cyanoethyl)glycine ethyl ester (prepared from methylaminopropionitrile and ethyl chloroacetate) in 1 liter of ethanol is hydrogenated in the presence of 60 g of Raney cobalt in an autoclave at a temperature of from 80° to 90°C and under a pressure of 100 to 120 atms. of hydrogen. The calculated quantity of hydrogen has been absorbed after about 1 hour. The hydrogenated solution is filtered off from the catalyst. The solid residue left after the ethanol has been evaporated is freed from any greases adhering to it by means of a little ethyl acetate, and the white product, which does not show any tendency towards discoloration in air, is fractionated in a high vacuum with 5 g of sodium methoxide. 424 g of 1-N-methyl-hexahydro-1,4-diazepin-3-one melting at 91°C are obtained. The calculated quantity of hydrogen has been absorbed after about 1 hour The hydrogenated solution is filtered off from the catalyst The solid residue left after the ethanol has been evaporated