HRID2236475

反应详情

EQUATION

反应方程式

HRID 2236475 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 3-Hydroxy-4-iodo-benzonitrile (300 mg, 1.22 mmol) in THF (5 mL) is added BH3.THF (10 mL, 1 M solution in THF, 10 mmol) under N2. The mixture is then allowed to stir at room temperature for 24 hours. The reaction is quenched with 6N HCl. THF is removed and the aqueous layer is neutralized with ammonium hydroxide to pH 9. The mixture is extracted with CHCl3/MeOH (9:1). The organic layer dried and evaporated and the residue is chromatographed to provide the desired product (60 mg, 20%). MS (ESI): 250 (M+1)−1.

WORKUP

后处理

  1. customThe reaction is quenched with 6N HCl
  2. customTHF is removed
  3. extractionThe mixture is extracted with CHCl3/MeOH (9:1)
  4. customThe organic layer dried
  5. customevaporated
  6. customthe residue is chromatographed