HRID923578

反应详情

EQUATION

反应方程式

HRID 923578 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirring solution of 4′-methyl-[1,1′-biphenyl]-4-carbonitrile (524 mg, 2.71 mmol) in DMF (10 mL) were added triethylamine (0.98 mL, 6.78 mmol) and hydroxylamine hydrochloride (471 mg, 6.78 mmol). After stirring at room temperature for 20 h, the reaction mixture was poured into NaHCO3 (50 mL), water (20 mL) and DCM (20 mL) then stirred for 20 min. The precipitate was isolated by filtration using water (2×10 mL) to wash the filter cake. The filter cake was then evaporated with toluene (2×5 mL) and dried under vacuum to afford 435 mg (70%) of N′-hydroxy-4′-methyl-[1,1′-biphenyl]-4-carboximidamide INT-40 as a white solid. LCMS-ESI (m/z) calculated for C14H14N2O: 226; found 227 [M+H]+, tR=1.34 min (Method 10).

WORKUP

后处理

  1. stirringthen stirred for 20 min
  2. customThe precipitate was isolated by filtration
  3. washto wash the filter cake
  4. customThe filter cake was then evaporated with toluene (2×5 mL)
  5. customdried under vacuum