HRID40393

反应详情

EQUATION

反应方程式

HRID 40393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyl (6-formyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate (400 mg, 1.44 mmol) and hydroxylamine hydrochloride (200 mg, 2.86 mmol) were combined in a flask with 25 mL of THF and 25 mL of 1 N NaOH solution. Stirred at rt for 1 h. Then added dichloromethane (50 mL) and extracted the aqueous layer 3 times with DCM (50 mL), dried over Na2SO4 and concentrated. Purified the oxime via MPLC (DCM/MeOH+1% NH4OH) to give title compound (200 mg, 47% yield) as a tan solid.

WORKUP

后处理

  1. extractionThen added dichloromethane (50 mL) and extracted the aqueous layer 3 times with DCM (50 mL)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customPurified the oxime via MPLC (DCM/MeOH+1% NH4OH)