反应 #355779

ord-7571bf433bdc40b49aa7e5a7ec38dfd3

反应方程式

CCn1ncnc1C=O
1-ethyl-1H-1,2,4-triazole-5-carbaldehyde
Cl.NO
hydroxylamine hydrochloride
O=C([O-])O.[Na+]
sodium bicarbonate
CCn1ncnc1C=NO
title compound
收率 31.1%
CCn1ncnc1C=NO
1-Ethyl-1H-1,2,4-triazole-5-carbaldehyde oxime
收率 31.1%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 3 hours
  3. 3
    温度After cooling
  4. 4
    过滤the reaction was filtered
  5. 5
    浓缩the filtrate concentrated in vacuo
  6. 6
    其他The resulting residue was crystallised from ethanol

实验过程

A mixture of crude 1-ethyl-1H-1,2,4-triazole-5-carbaldehyde (17.7 g), hydroxylamine hydrochloride (12.7 g, 0.182 mol), sodium bicarbonate (15.3 g, 0.182 mol) and ethanol (60 mL) was heated at reflux for 3 hours. After cooling, the reaction was filtered and the filtrate concentrated in vacuo. The resulting residue was crystallised from ethanol to give the title compound (6.17 g) 1H-NMR (d6-DMSO) δ 1.32 (3H, t, J=7 Hz), 4.41 (2H, q, J=7 Hz), 8.02 (1H, s), 8.25 (1H, s), 12.70 (1H, s)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07446117B2uspto-grants-2008_11