HRID1827538

反应详情

EQUATION

反应方程式

HRID 1827538 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of cyclohexanecarboxylic acid [2-chloro-4-(tetrahydro-pyran-2-yloxy)-benzyl]-[4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-amide (2.0 g) in 3:1 ethanol:1N HCl (40 mL) was stirred at room temperature for 1.5 hr. Saturated aqueous sodium bicarbonate solution was added and the aqueous solution was washed with methylene chloride. The organic solution was dried (magnesium sulfate), filtered and concentrated in vacuo. The crude product was purified by Biotage® chromatography (methylene chloride to 4% methanol/methylene chloride). The resulting white solid (1.53 g) was suspended in methanol (20 mL) and 4M HCl in dioxane was added. The mixture was stirred at room temperature for 1 hr. and was concentrated in vacuo to yield the title compound as a tan solid (1.60 g). MS 317.2 (MH+−40)

WORKUP

后处理

  1. washthe aqueous solution was washed with methylene chloride
  2. dry with materialThe organic solution was dried (magnesium sulfate)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by Biotage® chromatography (methylene chloride to 4% methanol/methylene chloride)
  6. addition4M HCl in dioxane was added
  7. concentrationand was concentrated in vacuo