HRID2068286

反应详情

EQUATION

反应方程式

HRID 2068286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 20 mL vial, ethyl 2-amino-1-cyclohexyl-1H-benzo[d]imidazole-5-carboxylate (101.5 mg, 0.0003532 mol) was dissoled in tetrahydrofuran (2 mL, 0.02 mol). While stirring under nitrogen, a solution of 1.0 M of lithium tetrahydroaluminate in tetrahydrofuran (1.0 mL) was added dropwise via a syringe to the reaction mixture. An initial reddish color occured followed by the reaction mixture becoming straw colored and a precipitate formed. After 1 hour the reaction was quenched by the dropwise addition of saturated ammonium chloride (1 mL). The mixture was extracted with ethyl acetate three times, the combined organic phases dried over sodium sulfate and concentrated to give the title compound (79.4 mg) as an off white solid.

WORKUP

后处理

  1. customa precipitate formed
  2. customAfter 1 hour the reaction was quenched by the dropwise addition of saturated ammonium chloride (1 mL)
  3. extractionThe mixture was extracted with ethyl acetate three times
  4. dry with materialthe combined organic phases dried over sodium sulfate
  5. concentrationconcentrated