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With benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; triethylamine; In dichloromethane; at 20℃; for 6h;
Intermediate 39: (4S, 10aR)-4-Aminohexahydropyrido[ 1 ,2-a] [ 1 ,4]diazepine- 1 ,5(2H,7H)- dioneA: (R)-Methyl l-((S)-2-(benzyloxycarbonylamino)-3-(tert- butoxycarbonylamino)propanoyl)piperidine-2-carboxylate[00284] To a suspension of (S)-2-(benzyloxycarbonylamino)-3-(tert- butoxycarbonylamino)propanoic acid (2.26 g, 6.68 mmol) in DCM (50 mL) was added (R)-methyl piperidine-2-carboxylate HC1 salt (1.00 g, 5.57 mmol), followed by EDC (1.60 g, 8.35 mmol), HOBT (1.71 g, 11.1 mmol), and TEA (2.33 mL, 16.7 mmol). The reaction mixture was stirred at rt for 6 hr. The reaction mixture was diluted with water and extracted with EtO Ac (2 x 30 mL). The combined EtOAc layers were washed with water and saturated aqueous NaCl, dried over Na2S04, filtered and concentrated. The crude product was purified using silica gel chromatography (ISCO system) eluting with a gradient of 30-70percent EtO Ac/Hex to give (R)-methyl l-((S)-2-(benzyloxycarbonylamino)- 3-(tert-butoxycarbonylamino)propanoyl)piperidine-2-carboxylate (1.80 g, 3.88 mmol, 69.8percent yield) as a white foam. Anal. Calcd. for C23H33N3O7 m/z 463.5, found: 464.3 (M+H)+.
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