1-amino-4-methylpentan-2-one;hydrochloride

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

実験手順: 2.75 g of isovalerylmethylamine hydrochloride, 3.8 g of sodium bicarbonate and 3.16 g of 4-fluorobenzoyl chloride are treated in the same manner as described in Preparation 1-(4). 4.0 g of N-(4-fluorobenzoyl)isovalerylmethylamine are thereby obtained. Yield: 82.9%. as described in Preparation 1-(4)

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

実験手順: 3.8 g of isovalerylmethylamine hydrochloride, 5.04 g of sodium bicarbonate and 4.9 g of 4-chlorobenzoyl chloride are treated in the same manner as described in Preparation 1-(4). 6.2 g of N-(4-chlorobenzoyl)isovalerylmethylamine are thereby obtained. Yield: 98.0. as described in Preparation 1-(4)

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Dissolve 1-amino-4-methyl-2-pentanone hydrochloride (1.4 g, 9.2 mmol) and potassium thiocyanate (1.3 g, 12.9 mmol) in water (3 mL). Stir the solution at 100° C. in a sealed flask for 2 h. Cool the mixture and concentrate in vacuo. Purify the residue by chromatography on silica gel (10 g) eluting with EtOAc to obtain a yellow solid (980 mg, estimated 1:1 product to starting material by NMR). Dissolve the yellow solid (980 mg) in water (2 mL) and concentrated hydrochloric acid (0.5 mL). Add potassium thiocyanate (0.7 g, 7.2 mmol) and heat the mixture at 100° C. for 16 h. Cool the mixture and concentrate in vacuo. Purify the residue by chromatography on silica gel (25 g) eluting with hexane/EtOAc (1:1) to obtain the title compound as a yellow solid (550 mg, 38%). MS (ES+) m/z: 157.2 (M+H)+. Cool the mixture concentrate in vacuo Purify the residue by chromatography on silica gel (10 g) eluting with EtOAc to obtain a yellow solid (980 mg, estimated 1:1 product to starting material by NMR) Cool the mixture concentrate in vacuo Purify the residue by chromatography on silica gel (25 g) eluting with hexane/EtOAc (1:1)

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

実験手順: Slurry 2-(4-methyl-2-oxo-pentyl)-isoindole-1,3-dione (2.8 g, 11.4 mmol) in concentrated HCl (18 mL), glacial acetic acid (16 mL) and water (13 mL). Stir the mixture at reflux for 16 h. Cool to room temperature and pour the solution onto ice (25 mL). Filter off the solids, wash the filtrate with cold water (20 mL) and concentrate in vacuo to a solid. Recrystallize the solid in ethanol (15 mL) and diethyl ether (50 mL). Decant off the solvent and dry the white paste under reduced pressure to obtain the desired intermediate as a white solid (1.4 g, 81%). at reflux for 16 h pour the solution onto ice (25 mL) Filter off the solids wash the filtrate with cold water (20 mL) concentrate in vacuo to a solid Recrystallize the solid in ethanol (15 mL) Decant off the solvent dry the white paste under reduced pressure

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

実験手順: 2.75 g of isovalerylmethylamine hydrochloride, 3.8 g of sodium bicarbonate and 3.16 g of 4-fluorobenzoyl chloride are treated in the same manner as described in Preparation 1-(4). 4.0 g of N-(4-fluorobenzoyl)isovalerylmethylamine are thereby obtained. Yield: 82.9%. as described in Preparation 1-(4)

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

実験手順: 3.8 g of isovalerylmethylamine hydrochloride, 5.04 g of sodium bicarbonate and 4.9 g of 4-chlorobenzoyl chloride are treated in the same manner as described in Preparation 1-(4). 6.2 g of N-(4-chlorobenzoyl)isovalerylmethylamine are thereby obtained. Yield: 98.0. as described in Preparation 1-(4)