HRID1585875

反应详情

EQUATION

反应方程式

HRID 1585875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl-2-hydroxy-4-iodo-benzoate from Step 2 (17.8 g, 64 mmol) was dissolved in THF. LiBH4 (3.07 g, 144 mmol) was added portionwise. The reaction mixture was heated at 50° for 16 hours. The reaction mixture was quenched carefully with 1N HCl and then extracted with EtOAc (3×). The organic layers were combined, washed with brine, dried (MgSO4) filtered and concentrated to yield the title compound as a white solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated at 50° for 16 hours
  2. customThe reaction mixture was quenched carefully with 1N HCl
  3. extractionextracted with EtOAc (3×)
  4. washwashed with brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated