HRID2271538

反应详情

EQUATION

反应方程式

HRID 2271538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of tert-butyl methyl(pyrrolidin-3-yl)carbamate (1.00 g, 5.0 mmol) in THF (25 mL) was added triethylamine (0.70 mL, 5.0 mmol) and 2-chloro-5-nitropyridine (500 mg, 3.15 mmol). The reaction mixture was then stirred at room temperature for 16 h, diluted with a saturated NaHCO3 solution and extracted with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and concentrated. Purification by column chromatography (silica, ethyl acetate/hexanes) afforded the desired product (1.02 g, 100%) as a yellow solid. ESI MS m/z 323 [C15H22N4O4+H]+

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customPurification by column chromatography (silica, ethyl acetate/hexanes)