HRID239949

反应详情

EQUATION

反应方程式

HRID 239949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of aqueous 2N NaOH (2.00 ml) is added to a stirred solution of ethyl 3,5-dimethyl-4-[[2-methyl-5-(4-oxo-1-piperidyl)benzoyl]amino]benzoate (0.11 g, 269.28 μmol) in THF:MeOH (2.4 ml:1.2 ml). After 16 hours at ambient temperature, the organic solvent is removed under reduced pressure and the residue is diluted with water, acidified to pH 7 with 1N HCl, and extracted twice with ethyl acetate. The organic layers are combined with aqueous layer and concentrated under reduced pressure. The resulting solids are triturated with 1:1 mixture of acetonitrile and ethanol to give white slurry that is filtered through Celite™ bed. The filtrate is concentrated under reduced pressure and the precipitate is triturated with acetone and filtered to afford the title compound as an off-white solid (99 mg, 99%). Mass spectrum (m/z): 381.2 (M+1).

WORKUP

后处理

  1. customthe organic solvent is removed under reduced pressure
  2. additionthe residue is diluted with water
  3. extractionextracted twice with ethyl acetate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting solids are triturated with 1:1 mixture of acetonitrile and ethanol
  6. customto give white slurry that
  7. filtrationis filtered through Celite™ bed
  8. concentrationThe filtrate is concentrated under reduced pressure
  9. customthe precipitate is triturated with acetone
  10. filtrationfiltered