HRID1605249

反应详情

EQUATION

反应方程式

HRID 1605249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 11.20 g (0.04 mole) of [4-(p-anisidino)-6-methyl-2-pyrimidinylthio]acetonitrile, 5.52 g (0.08 mole) of hydroxylamine hydrochloride and 16.90 g (0.16 mole) of sodium carbonate in 150 ml of N,N-dimethylformamide was heated on a steam bath for three and one-half hours. The mixture was filtered and the filtrate was evaporated in a rotary evaporator. The residue was dissolved in ethyl acetate, diluted with petroleum ether and was cooled in ice. The precipitate which formed was collected and recrystallized from a mixture of ethanol-petroleum ether to afford 3.7 g of product, m.p. 189°-191° d.

WORKUP

后处理

  1. temperaturewas heated on a steam bath for three and one-half hours
  2. filtrationThe mixture was filtered
  3. customthe filtrate was evaporated in a rotary evaporator
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. additiondiluted with petroleum ether
  6. temperaturewas cooled in ice
  7. customThe precipitate which formed
  8. customwas collected
  9. customrecrystallized from a mixture of ethanol-petroleum ether