HRID2244012

反应详情

EQUATION

反应方程式

HRID 2244012 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1-[2-hydroxy-4-(4-nitro-benzyloxy)-3-propyl-phenyl]-ethanone (1.0 g, 3.0 mmol) in tetrahydrofuran (13 mL) is added concentrated hydrochloric acid (2.7 mL) and stannous chloride dihydrate (2.2 g, 9.9 mmol). The reaction mixture is stirred at room temperature overnight. The reaction mixture is quenched into saturated aqueous NH4Cl (100 mL). The resulting emulsion is filtered and the filtrate extracted with ethyl acetate (3×100 mL). The combined organic layers are washed with brine, dried over sodium sulfatesodium sulfate, and concentrated to provide the title compound in crude form (980 mg,). LC-MS (m/z): 298 (M−1).

WORKUP

后处理

  1. customThe reaction mixture is quenched into saturated aqueous NH4Cl (100 mL)
  2. filtrationThe resulting emulsion is filtered
  3. extractionthe filtrate extracted with ethyl acetate (3×100 mL)
  4. washThe combined organic layers are washed with brine
  5. dry with materialdried over sodium sulfatesodium sulfate
  6. concentrationconcentrated