HRID1605249
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated on a steam bath for three and one-half hours
- filtrationThe mixture was filtered
- customthe filtrate was evaporated in a rotary evaporator
- dissolutionThe residue was dissolved in ethyl acetate
- additiondiluted with petroleum ether
- temperaturewas cooled in ice
- customThe precipitate which formed
- customwas collected
- customrecrystallized from a mixture of ethanol-petroleum ether