HRID2088936

反应详情

EQUATION

反应方程式

HRID 2088936 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Combine tert-butyl 4-(4,5-diiodo-1-(2-(pyrrolidin-1-yl)ethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate (51.00 g, 84.96 mmol) and 2-methyltetrahydrofuran (357 mL). Cool the reaction mixture to 0° C. Add 2 M isopropylmagnesium chloride in tetrahydrofuran (55.22 mL, 1.3 eq) dropwise over 45 minutes, maintaining the temperature below 5° C. Add saturated aqueous ammonium chloride. Separate the layers. Wash the aqueous phase with methyl tert-butyl ether. Wash the organics with aqueous saturated sodium chloride. Dry the organics over anhydrous magnesium sulfate, decolor with charcoal, filter, and concentrate in vacuo to give tert-butyl 4-(4-iodo-1-(2-(pyrrolidin-1-yl)ethyl)-1H-imidazol-2-yl)piperidine-1-carboxylate as a yellow solid (39.50 g, 98%). MS (ES) m/z=475 [M]+.

WORKUP

后处理

  1. temperaturemaintaining the temperature below 5° C
  2. customSeparate the layers
  3. washWash the aqueous phase with methyl tert-butyl ether
  4. washWash the organics with aqueous saturated sodium chloride
  5. dry with materialDry the organics over anhydrous magnesium sulfate, decolor with charcoal
  6. filtrationfilter
  7. concentrationconcentrate in vacuo