HRID323344

反应详情

EQUATION

反应方程式

HRID 323344 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine (1-(t-butoxycarbonyl)-1H-benzimidazol-2-yl)(1-(t-butoxycarbonyl)piperidin-4-yl)amine (3.2 g, 7.7 mmol), tetrahydrofuran/water (200 mL/200 mL). Add a 1 M aqueous solution of sodium hydroxide (8.4 mL, 8.4 mmol). Heat to reflux. After 18 hours, concentrate the reaction mixture in vacuo to form a solid. Dillute with water, adjust the pH to about 7 using a 1 M aqueous solution of hydrochloric acid, collect the solid by filtration, and dry to give (1H-benzimidazol-2-yl)(1-(t-butoxycarbonyl)piperidin-4-yl)amine: Rf=0.38 (silica gel, 20/1 ethyl acetate/methanol).

WORKUP

后处理

  1. temperatureHeat to reflux
  2. concentrationconcentrate the reaction mixture in vacuo
  3. customto form a solid
  4. customcollect the solid
  5. filtrationby filtration
  6. customdry