HRID473231

反应详情

EQUATION

反应方程式

HRID 473231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Aminomethyl-6-[(tert-butyldimethylsilyloxy)methyl]pyridine (26) (380 mg, 1.50 mmol) and 1,1′-carbonyldiimidazole (150 mg, 0.92 mmol) were suspended in THF (10 mL). The air was evacuated from the reaction system, and then Ar was charged therein. The suspension was stirred for 24 hours at a room temperature. TLC was used to confirm there was no starting material in the mixture. Then, the reaction mixture was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (CDCl3:MeOH=50:1) to give N,N′-bis{[6-(tert-butyldimethylsilyloxy)methylpyridin-2-yl]methyl}urea (27) (384 mg, 96%) as yellow crystals.

WORKUP

后处理

  1. customThe air was evacuated from the reaction system
  2. additionAr was charged
  3. customThen, the reaction mixture was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (CDCl3:MeOH=50:1)