HRID1089832

反应详情

EQUATION

反应方程式

HRID 1089832 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-methoxy-9-fluorenecarboxylic acid (2.2 g, 9.2 mmol) in 100 mL of THF at 0° C. was charged with 1M THF solution of BH3 -THF complex (20 mL, 20 mmol). The reaction mixture was stirred overnight then quenched with 10 mL of 10% acetic acid in methanol an diluted with 100 mL of water. The layers were separated, the aqueous phase was extracted with ethyl acetate (3×25 mL). The combined extracts were dried over magnesium sulfate and evaporated. The residue was crystallized from methanol-water to afford 1.87 g (87.0%) of product.

WORKUP

后处理

  1. customthen quenched with 10 mL of 10% acetic acid in methanol
  2. additionan diluted with 100 mL of water
  3. customThe layers were separated
  4. extractionthe aqueous phase was extracted with ethyl acetate (3×25 mL)
  5. dry with materialThe combined extracts were dried over magnesium sulfate
  6. customevaporated
  7. customThe residue was crystallized from methanol-water