HRID547382

反应详情

EQUATION

反应方程式

HRID 547382 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 2,3-diaminopyridine in tetrahydrofuran/pyridine (10/1) at 0° C. benzylchloroformate was added dropwise. The suspension was stirred at room temperature and after 2 hours partitioned between water and EtOAc. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic phases were dried over sodium sulfate and the filtrate concentrated to dryness under reduced pressure. To the residue was added Et2O-MeOH and the solid was filtered.

WORKUP

后处理

  1. custompartitioned between water and EtOAc
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with EtOAc
  4. dry with materialThe combined organic phases were dried over sodium sulfate
  5. concentrationthe filtrate concentrated to dryness under reduced pressure
  6. additionTo the residue was added Et2O-MeOH
  7. filtrationthe solid was filtered