HRID1985210

反应详情

EQUATION

反应方程式

HRID 1985210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customConcentration of the reaction mixture gave an oil which
  2. customis partitioned between ethyl acetate (20 ml) and water (25 ml)
  3. washThe ethyl acetate layer is washed with water (15 ml), brine (20 ml)
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated to an oil which
  6. customis purified by chromatography on a Biotage silica cartridge (gradient elution, 100% methylene chloride to 10:1 methylene chloride:methanol)