反应详情

温度

0 °C

To a solution of (±)-{3-[(3-benzyl-5-chloro-4-oxo-3,4-dihydro-pyrrolo[2,1-f][1,2,4]triazin-2-ylmethyl)-amino]-propyl}-carbamic acid tert-butyl ester (12 mg, 0.027 mmole) in methylene chloride (0.5 mL) at 0° C. was added Et3N (11 μL, 0.081 mmole) followed by 4-chlorobenzoyl chloride (10 mL, 0.081 mmol). After stirring at 0° C. for 1.5 h, the reaction was quenched with 10 mL of saturated NaHCO3 solution and extracted with EtOAc (3×20 mL). The pooled organic extracts were dried over anhydrous MgSO4 and concentrated in vacuo. Purification of the residue by flash column chromatography (SiO2, 2% MeOH/CHCl3) gave a residue which was immediately treated with 4 N HCl in dioxane (1 mL). The crude product was lyophilized with acetonitrile/water to give the title compound as a white powder (7.2 mg, 51%): MS (ESI+) 484 (M++H).

1. customthe reaction was quenched with 10 mL of saturated NaHCO3 solution
2. extractionextracted with EtOAc (3×20 mL)
3. dry with materialThe pooled organic extracts were dried over anhydrous MgSO4
4. concentrationconcentrated in vacuo
5. customPurification of the residue by flash column chromatography (SiO2, 2% MeOH/CHCl3)
6. customgave a residue which