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HRID1904080

反应详情

EQUATION

反应方程式

HRID 1904080 的结构方程式

REACTANTS

反应物

2
结构：Cc1ccc(Cc2cnc(N[N+](=O)[O-])[nH]c2=O)cn1
HCID3018360

N-{4-Hydroxy-5-[(6-methylpyridin-3-yl)methyl]pyrimidin-2-yl}nitramide

C11H11N5O3

结构：CN(C)Cc1ccnc(CSCCN)c1
HCID13277327

未命名化合物

PRODUCTS

生成物

1
结构：Cc1ccc(Cc2cnc(NCCSCc3cc(CN(C)C)ccn3)[nH]c2=O)cn1
HCID13292604

未命名化合物

收率 61.6%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：c1ccncc1
溶剂HCID1049

Pyridine

C5H5N

PROCEDURE

实验过程

A solution of 2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine (0.5 g) and 2-nitroamino-5-(6-methyl-3-pyridylmethyl)-4-pyrimidone (0.7 g) in pyridine (3 ml) was heated under reflux for 3.5 hours and evaporated to dryness. The residue was purified by elution from a column of silica gel with ethyl acetate:ethanol: 28% w/w aqueous ammonia (by volume 10:15:2) and recrystallisation from acetonitrile to give 2-[2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamino]-5-(6-methyl-3-pyridylmethyl)-4-pyrimidone (0.58 g) m.p. 128°-129.5°.

WORKUP

后处理

  1. temperatureunder reflux for 3.5 hours
  2. customevaporated to dryness
  3. customThe residue was purified by elution from a column of silica gel with ethyl acetate
  4. customethanol: 28% w/w aqueous ammonia (by volume 10:15:2) and recrystallisation from acetonitrile