HRID1985210
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of the ester obtained in Step A (70 mg, 0.10 mmol) in trifluoroacetic (1 ml) and methylene chloride (2 ml) is stirred at 23° C. for 7 hours. Concentration of the reaction mixture gave an oil which is partitioned between ethyl acetate (20 ml) and water (25 ml). The ethyl acetate layer is washed with water (15 ml), brine (20 ml), dried (Na2SO4), and concentrated to an oil which is purified by chromatography on a Biotage silica cartridge (gradient elution, 100% methylene chloride to 10:1 methylene chloride:methanol) to produce an oil (31 mg, 48%).
WORKUP
后处理
- customConcentration of the reaction mixture gave an oil which
- customis partitioned between ethyl acetate (20 ml) and water (25 ml)
- washThe ethyl acetate layer is washed with water (15 ml), brine (20 ml)
- dry with materialdried (Na2SO4)
- concentrationconcentrated to an oil which
- customis purified by chromatography on a Biotage silica cartridge (gradient elution, 100% methylene chloride to 10:1 methylene chloride:methanol)