反应详情

To a solution of (R)-3-(benzyloxy)-2-(2-(tert-butoxycarbonylamino)-2-methyl propanamido) propanoic acid (Intermediate 3A) ((280 mg, 0.736 mmol) and 2-methyl-4-phenyl-2,7-diazaspiro[4.4]nonan-1-one (step 2) (170 mg, 0.736 mmol)) in DMF (5 mL) was added DIPEA (514 uL, 2.94) and followed by ®T3P (amide coupling agent 50% in DMF, 859 uL, 1.47 mmol). The reaction was stirred at room temperature over 3 days. The resulting mixture was diluted with water (50 ml) and extracted with EtOAc (2×100 ml). The combined organic extracts were dried (MgSO4) and concentrated in vacuo. Purification by chromatography on silica eluting with TBME:MeOH afforded the title compound

1. extractionextracted with EtOAc (2×100 ml)
2. dry with materialThe combined organic extracts were dried (MgSO4)
3. concentrationconcentrated in vacuo
4. customPurification by chromatography on silica eluting with TBME