HRID928415

反应详情

EQUATION

反应方程式

HRID 928415 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(4-hydroxymethyl-benzyl)-1H-[1,2,3]triazole-4-carboxylic acid (0.95 g, 4.07 mmol), (5-Aminomethyl-4,6-dimethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.024 g, 4.07 mmol), HATU (2.013 g, 5.30 mmol) and DIPEA (2.85 mL, 16.29 mmol) in 50 mL DMF was stirred at room temperature for 3 h. The reaction mixture was concentrated under reduced pressure. The residue was taken up in ethyl acetate and washed with 1 n HCl solution and saturated sodium bicarbonate solution. The organic solution was dried over MgSO4, filtered and concentrated to yield the crude product which was used in the next step without further purification. LCMS (Method A) RtA=1.279; [M+H]+=467.0.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. washwashed with 1 n HCl solution and saturated sodium bicarbonate solution
  3. dry with materialThe organic solution was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated