HRID1498066

反应详情

EQUATION

反应方程式

HRID 1498066 的结构方程式

PROCEDURE

实验过程

Triethylsilane (0.160 mL, 1.00 mmol) was added to a solution of 1.45 g (2.36 mmol) of methyl 6-iodo-5-(2-(1-trityl-1H-imidazol-2-yl)ethoxy)nicotinate in trifluoroacetic acid (30.0 mL, 389 mmol). The mixture was stirred for 4 hours, concentrated in vacuum and triturated with 50 ml of anhydrous ethyl ether. The solid material was collected, washed with several portions of ether and partitioned between 1 M of aqueous sodium carbonate and ethyl acetate. The organic extracts were washed with water, brine, dried over magnesium sulfate and concentrated in vacuum to give a residue (0.55 g, 62%) of methyl 5-(2-(1H-imidazol-2-yl)ethoxy)-6-iodonicotinate. MS(ESI+): 374.0

WORKUP

后处理

  1. concentrationconcentrated in vacuum
  2. customtriturated with 50 ml of anhydrous ethyl ether
  3. customThe solid material was collected
  4. washwashed with several portions of ether
  5. custompartitioned between 1 M of aqueous sodium carbonate and ethyl acetate
  6. washThe organic extracts were washed with water, brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated in vacuum