反应详情

To a 1.8 M solution of 5-amino-2-methylthio-4-(3-methoxyphenyl)-quinazoline-6-carboxylic acid in DMF (1.8 ml) were added TBTU (173 mg) and tert-butylamine (95 l). The reaction mixture was stirred for 2 h and then poured into a mixture of EtOAc (25 ml) and saturated aqueous NaHCO3 (50 ml). The organic phase was separated and washed with 0.5 M aqueous HCl (50 ml) and brine (50 ml), followed by drying (MgSO4) and concentration under reduced pressure. The title compound was purified by chromatography on silica gel using hept/EtOAc=1/0 to 2/3 (v/v) as the eluent. The title compound was lyophilized from a mixture of dioxane and water containing 1.5 equiv. of HCl.

1. customThe organic phase was separated
2. washwashed with 0.5 M aqueous HCl (50 ml) and brine (50 ml)
3. customby drying
4. concentration(MgSO4) and concentration under reduced pressure
5. customThe title compound was purified by chromatography on silica gel using hept/EtOAc=1/0 to 2/3 (v/v) as the eluent