反应详情

N-(tert-butoxycarbonyl)-N-methyl-β-alanine (Matrix Scientific, 368 mg, 1.81 mmol) was dissolved in N,N-dimethylformamide (3.7 mL) and treated with N,N-carbonyldiimidazole (308 mg, 1.90 mmol). The reaction mixture was stirred at room temperature for 30 minutes. (4-Aminobutyl)(triphenyl)phosphonium bromide (1.12 g, 2.72 mmol) was added, and the reaction was stirred overnight at room temperature. The reaction was then diluted with methylene chloride and washed with 5% aqueous lithium chloride (3 times), 1N aqueous hydrogen chloride, and saturated sodium bicarbonate. The organic solution was dried over anhydrous sodium sulfate, filtered, and concentrated to give the title compound (1.26 g, 100%, 86% pure) as a white foam. Sample was used crude in next step.

1. stirringthe reaction was stirred overnight at room temperature
2. washwashed with 5% aqueous lithium chloride (3 times), 1N aqueous hydrogen chloride, and saturated sodium bicarbonate
3. dry with materialThe organic solution was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated