反应详情

温度

100 °C

A solution of methyl 5-bromo-2-{[2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)ethyl]oxy}benzoate (Preparation 70) (8.92 g, 23.8 mmmol) in DCM (18 ml) was treated with TFA (7 ml) and stirred for 5 hrs. Additional (2 ml) TFA was added and the reaction left overnight. The solvent was evaporated, re-evaporated with toluene (5×) and dissolved in toluene (50 ml). The resulting residue was treated with triethylamine (4 equiv) and heated at 100° C. overnight then evaporated. The residue was purified by flash chromatography twice eluting with 50% EtOAc/hexane then 40-45% EtOAc/hexane. The fractions were evaporated to give the title compound (3.4 g) as a white solid. MS (ES): C9H881BrNO2 requires 243; found 244 [M+H]+.

1. waitthe reaction left overnight
2. customThe solvent was evaporated
3. customre-evaporated with toluene (5×)
4. dissolutiondissolved in toluene (50 ml)
5. customthen evaporated
6. customThe residue was purified by flash chromatography
7. washtwice eluting with 50% EtOAc/hexane
8. customThe fractions were evaporated