HRID875203

反应详情

EQUATION

反应方程式

HRID 875203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (1-methyl-1H-imidazol-2-yl)(phenyl)methanone (20.8 g, 112 mmol) and hydroxylamine hydrochloride (19.4 g, 279 mmol) in pyridine (120 mL) was stirred 8 h at 50° C. then overnight at room temperature. After removal of the solvent in vacuo, addition of water (500 mL) induced precipitation of a white solid that was filtered off, washed with water (2×50 mL) and dried. A second filtration of the liquor yielded a second crop of solid. The combined crops afforded N-hydroxy-1-(1-methyl-1H-imidazol-2-yl)-1-phenylmethanimine [18.5 g, yield 80%; HPLC/MS: m/z=202 (M+H); log P(HCOOH)=0.24].

WORKUP

后处理

  1. customovernight
  2. customat room temperature
  3. customAfter removal of the solvent
  4. additionin vacuo, addition of water (500 mL)
  5. customprecipitation of a white solid
  6. filtrationthat was filtered off
  7. washwashed with water (2×50 mL)
  8. customdried
  9. filtrationA second filtration of the liquor
  10. customyielded a second crop of solid