HRID5003

反应详情

EQUATION

反应方程式

HRID 5003 的结构方程式

PROCEDURE

实验过程

200 Grams of 6-chloroacetylaminomethyl-2,3-dihydro-7-hydroxy-4-methyl-1H-indene-1-one, 77.9 g of hydroxylamine hydrochloride, 300 ml of pyridine and 1,800 ml of ethanol were refluxed for 3 hours. After the reaction was completed, the solvent was removed by evaporation under a reduced pressure, then to the residue thus obtained was added 2 liters of water and the mixture was stirred vigorously, cooled and crystallized. The crystals were collected by filtration, washed with water, and recrystallized from water to obtain 167 g of (2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6yl)-methylaminocarbonylmethylpyridinium chloride. Colorless flake-like crystals. Melting point: 279° C. (Decomposed).

WORKUP

后处理

  1. customthe solvent was removed by evaporation under a reduced pressure
  2. customto the residue thus obtained
  3. temperaturecooled
  4. customcrystallized
  5. filtrationThe crystals were collected by filtration
  6. washwashed with water
  7. customrecrystallized from water