3-N-BOC-AMINO-4,4-DIMETHYL PENTANOIC ACID synthesis

Yield:856417-59-9 85%

Reaction Conditions:

with triethylamine in tetrahydrofuran;water at 20; for 15 h;

Steps:

47.a 47a)

47a) 3-((tert-butoxycarbonyl)amino)-4,4-dimethylpentanoic acid 3-amino-4,4-dimethylpentanoic acid (0.51 g) and triethylamine (0.78 g) were dissolved in THF (10 ml) and water (10 ml), di-tert-butyl dicarbonate (0.71 g) was added thereto, and mixed at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, washed with diethyl ether, acidified with a 5% aqueous citric acid solution, and then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to obtain the title compound as colorless powder (0.65 g, 85%). NMR (CDCl₃) δ: 0.93 (9H, s), 1.43 (9H, s), 2.60-2.67 (2H, m), 4.69-4.72 (1H, m), 5.54-5.56 (1H, m).

References:

EP1695961,2006,A1 Location in patent:Page/Page column 59-60