HRID2366478

反应详情

EQUATION

反应方程式

HRID 2366478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(1-(tert-butoxycarbonyl)piperidin-4-yl)benzoic acid (0.7 g, 2.3 mmol), N,O-dimethylhydroxylamine (0.27 g, 2.8 mmol), 1-hydroxybenzotriazole (0.37 g, 2.7 mmol) and 1-ethyl-3-[3-dimethylaminopropyl]carbodiimide hydrochloride (1.1 g, 5.8 mmol) in tetrahydrofuran (15 mL) was stirred at ambient temperature for 48 hours. Additional N,O-dimethylhydroxylamine (0.14 g, 1 mmol) was added and the mixture stirred an additional 4 hours and concentrated. The residue was dissolved in ethyl acetate, washed with water and filtered through silica gel. The solution was concentrated and used without further purification.

WORKUP

后处理

  1. stirringthe mixture stirred an additional 4 hours
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water
  5. filtrationfiltered through silica gel
  6. concentrationThe solution was concentrated
  7. customused without further purification