HRID1666341

反应详情

EQUATION

反应方程式

HRID 1666341 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 1H-benzo[d][1,2,3]triazol-5-amine (1.85 g, 13.8 mmol, Alfa Aesar) in THF (10 mL) and CH3CN (8 mL) was added pyridine (1.34 mL, 16.6 mmol) followed by phenyl chloroformate (2.27 mL, 14.5 mmol) slowly. The reaction was stirred overnight. The reaction was concentrated to give an oil, which was partitioned between CH2Cl2 and water. The organic layer was dried using a SPE phase separator and concentrated to give a solid. This was taken up in CH2Cl2 and the precipitate was filtered to give the desired product (2.0 g, 57%) which was used without purification. MS M+1: 256.06.

WORKUP

后处理

  1. concentrationThe reaction was concentrated
  2. customto give an oil, which
  3. customwas partitioned between CH2Cl2 and water
  4. customThe organic layer was dried
  5. concentrationconcentrated
  6. customto give a solid
  7. filtrationthe precipitate was filtered