HRID1071452

反应详情

EQUATION

反应方程式

HRID 1071452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Butylamine (30 mL, 300 mmol) was dissolved in 150 mL of acetonitrile at room temperature. 2-Chloromethylbenzimidazole (5 g, 30 mmol) dissolved in 50 mL dimethylformamide was added dropwise. After stirring 3 hours at room temperature, the solvent was removed in vacuo. The residue was dissolved in 100 mL ethyl acetate and washed 2×100 mL H2O followed by 1×100 mL brine. The organic layer was dried over MgSO4, filtered, and then concentrated. The residue was purified by silica gel chromatography eluting first with ethyl acetate then with 10/2/1 ethyl acetate/methanol/triethylamine to yield 2.6 g 2-butylaminomethylbenzimidazole.

WORKUP

后处理

  1. additionwas added dropwise
  2. customthe solvent was removed in vacuo
  3. dissolutionThe residue was dissolved in 100 mL ethyl acetate
  4. washwashed 2×100 mL H2O
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by silica gel chromatography
  9. washeluting first with ethyl acetate