HRID2235235

反应详情

EQUATION

反应方程式

HRID 2235235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Suspend 2,6-dichloro-4-hydroxy-benzaldehyde in 3 L EtOH and cool in an ice bath at 0° C. Add 32.97 g (871.45 mmol) NaBH4 caplets portionwise. Remove the ice bath and stir for 2 hours. Carefully add the reaction mixture to 8 L sat'd. NH4Cl solution and stir until fully quenched. Extract with CH2Cl2 (2×2 L) and dry the combined organic extracts over Na2SO4. Filter and concentrate under vacuum to yield 247 g (100%) of (4-benzyloxy-2,6-dichloro-phenyl)methanol as a white solid.

WORKUP

后处理

  1. customRemove the ice bath
  2. additionCarefully add the reaction mixture to 8 L
  3. stirringNH4Cl solution and stir
  4. customuntil fully quenched
  5. extractionExtract with CH2Cl2 (2×2 L)
  6. dry with materialdry the combined organic extracts over Na2SO4
  7. filtrationFilter
  8. concentrationconcentrate under vacuum