HRID2105883

反应详情

EQUATION

反应方程式

HRID 2105883 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-tert-butyloxycarbonyl-1-[2-(tert-butyldimethylsilyloxy)ethyl]-piperazin-2-one (0.88 g, 2.5 mmol) in tetrahydrofuran (30 mL) was added tetrabutylammonium fluoride (3.6 mL, 3.6 mmol, 1.0 M in tetrahydrofuran) and the reaction mixture was stirred at room temperature for 2 h. The reaction mixture was quenched with a dilute aqueous solution of sodium bicarbonate and extracted with ethyl acetate. The organic extracts were washed with brine and dried over anhydrous sodium sulfate. Purification of the crude residue by flash column chromatography (silica gel, eluting with 30% ethyl acetate in hexanes) gave 4-tert-butyloxycarbonyl-1-(2-hydroxyethyl)-piperazin-2-one (0.45 g, 75%).

WORKUP

后处理

  1. customThe reaction mixture was quenched with a dilute aqueous solution of sodium bicarbonate
  2. extractionextracted with ethyl acetate
  3. washThe organic extracts were washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customPurification of the crude residue
  6. washby flash column chromatography (silica gel, eluting with 30% ethyl acetate in hexanes)