HRID1670899

反应详情

EQUATION

反应方程式

HRID 1670899 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dess-Martin periodinane (450 mg, 1.06 mmol) was added to a solution of hydroxy-di-thiophen-2-yl-acetic acid (1S,2R,4S,7S)-7-[(9-hydroxy-nonyl)-methyl-amino]-bicyclo[2.2.1]hept-2-yl ester (370 mg, 0.732 mmol) in dry DCM (3 mL) at 0° C., and the reaction mixture allowed to warm to RT. After 1 h at RT the reaction mixture was treated with satd NaHCO3 (aq) and extracted with ethyl acetate. The organic layer was washed with brine, dried (Na2SO4), filtered, and concentrated to dryness. The residue was triturated with ether, and the solids removed by filtration. The filtrate was concentrated to afford an orange/brown viscous oil and used directly without further purification.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe residue was triturated with ether
  7. customthe solids removed by filtration
  8. concentrationThe filtrate was concentrated
  9. customto afford an orange/brown viscous oil
  10. customused directly without further purification