HRID49455

反应详情

EQUATION

反应方程式

HRID 49455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Commercially available 2-amino-9-fluorenone 1 (10 mmol) was dissolved in 100 mL of methanol and 0.38 g (10 mmol) of sodium borohydride was added. The mixture was stirred at 25° C. for 1 h and concentrated to dryness under vacuum. The residue was suspended in 100 mL of saturated aqueous NaHCO3− and extracted with ethylacetate (100 mL). The ethylacetate layer was concentrated under vacuum and the residue was crystallized from ethylacetate/hexane (2:1) to afford 1.4 g of pure 2-amino-9-hydroxyfluorene 2.

WORKUP

后处理

  1. concentrationconcentrated to dryness under vacuum
  2. extractionextracted with ethylacetate (100 mL)
  3. concentrationThe ethylacetate layer was concentrated under vacuum
  4. customthe residue was crystallized from ethylacetate/hexane (2:1)