反应详情

温度

90 °C

To a stirred solution of (v) (20 g, 0.06 mol) in EtOH:water (400 ml, 1:1 v/v) was added NaOH (59.0 g, 0.02 mol) and the reaction mixture heated at 90° C. for 15 h. The reaction was then cooled to RT and the volatiles were removed in vacuo. The residual aqueous solution was acidified to pH 2 with aq. 2N HCl solution whereupon a solid precipitated from solution. The solid was separated by filtration and dissolved in EtOAc (300 mL), dried (Na2SO4) and concentrated in vacuo to give (vi) (7.5 g, with purity 75% by HPLC analysis). The material was used unpurified in subsequent steps.

1. temperatureThe reaction was then cooled to RT
2. customthe volatiles were removed in vacuo
3. customprecipitated from solution
4. customThe solid was separated by filtration
5. dissolutiondissolved in EtOAc (300 mL)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo