反应详情

To a solution of compound 12 (0.13 mmol) in THF (2 mL), was added a large excess of NaHCO3 (s) and a solution of phosgene in toluene (1.6 M, 600 μL). After 10 min of agitation the slurry was filtered and concentrated to dryness. The solid was redissolved in dichloromethane and a large excess of NaHCO3 (s) and 2-Amino-N-(2-hydroxy-indan-1-yl)-3,3-dimethyl-butyramide (0.65 mmol) was added. The slurry was agitated for 24-40 hrs at RT. The slurry was filtered, concentrated and subjected to silica column chromatography (gradient elution from 100% DCM to MeOH/DCM 2:98) to give the title compound (89.6 mg, 0.11 mmol). Purity by HPLC>95%. M+H+790.3.

1. filtrationAfter 10 min of agitation the slurry was filtered
2. concentrationconcentrated to dryness
3. dissolutionThe solid was redissolved in dichloromethane
4. filtrationThe slurry was filtered
5. concentrationconcentrated
6. washsubjected to silica column chromatography (gradient elution from 100% DCM to MeOH/DCM 2:98)