HRID1526767

反应详情

EQUATION

反应方程式

HRID 1526767 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 the product from example H (2 gm, 5.204 mmol) in 1,4-Dioxane (20 ml) was added saturated aq. NaHCO3 solution (2.5 ml) and stirred for 5 min at RT. Boc-anhydride (1.36 ml, 6.245 mmol) was then added to it at 0 C and the reaction mixture was allowed to stir at room temperature for 2 hrs. Reaction mixture was concentrated, dissolved in EtOAc (60 ml) and washed with water (60 ml), dried over Na2SO4, filtered and concentrated under reduced pressure to obtain the crude which was purified by silica gel (100-200 mesh) column chromatography eluting with 10% EtOAc to afford the desired compound (1.7 g) as a colorless liquid.

WORKUP

后处理

  1. stirringto stir at room temperature for 2 hrs
  2. customReaction mixture
  3. concentrationwas concentrated
  4. dissolutiondissolved in EtOAc (60 ml)
  5. washwashed with water (60 ml)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customto obtain the crude which
  10. customwas purified by silica gel (100-200 mesh) column chromatography
  11. washeluting with 10% EtOAc