HRID1363387

反应详情

EQUATION

反应方程式

HRID 1363387 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 compound of example 106 (3.35 g, 7.79 mmol) in dry CHCl3 (25 mL) was added acetic anhydride (1.76 g, 17.43 mmol) at 25° C. with stirring, followed by the addition of dimethylaminopyridine (0.033 g, 1% w/w). The mixture was stirred for 0.5 h. It was poured into ice water (50 mL), basified using a saturated aqueous Na2CO3 solution and extracted using CHCl3 (3×100 mL). The organic extract was washed with water, dried (anhydrous Na2SO4) and concentrated. The oil obtained was purified using a silica gel column and 0.1% MeOH+1% liquor NH3 in CHCl3 as eluant to get the title compound.

WORKUP

后处理

  1. stirringThe mixture was stirred for 0.5 h
  2. extractionextracted
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried (anhydrous Na2SO4)
  6. concentrationconcentrated
  7. customThe oil obtained
  8. customwas purified