HRID1727258

反应详情

EQUATION

反应方程式

HRID 1727258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N,N-carbonyldiimidazole (2.1 g, 12.8 mmol) in THF (15 mL) was added a solution of 3-pyridylcarbinol (1.3 g, 11.6 mmol) in THF (15 mL). After stirring for 30 minutes, a solution of (4-aminomethylphenyl)methanol (1.4 g, 10.4 mmol) in THF (15 mL) and triethylamine (3.2 mL, 23.2 mmol) were added, and the mixture was stirred overnight. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with water (30 mL) and extracted with 10% MeOH in CHCl3 (30 mL×2). The organic layer was dried (Na2SO4), evaporated under reduced pressure, and the residue was purified by MPLC on silica gel (5% MeOH in CHCl3) to afford the titled compound (1.31 g, 46%) as a white solid.

WORKUP

后处理

  1. stirringthe mixture was stirred overnight
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionthe residue was diluted with water (30 mL)
  4. extractionextracted with 10% MeOH in CHCl3 (30 mL×2)
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. customevaporated under reduced pressure
  7. customthe residue was purified by MPLC on silica gel (5% MeOH in CHCl3)