反应 #1256769

ord-07baa239dfbb4c0dbda1d0ce5446d3e4

反应方程式

O=Cc1cnccc1Cl
4-Chloro-pyridine-3-carbaldehyde
[Na+].[OH-]
NaOH
O
H2O
Cl.NO
hydroxylamine hydrochloride
ON=Cc1cnccc1Cl
4-Chloro-pyridine-3-carbaldehyde Oxime

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他White crystals precipitated
  2. 2
    过滤were collected by filtration
  3. 3
    洗涤washed with H2O (30 ml)
  4. 4
    其他The product was dried 1 h at 50° C. on the high vacuum
  5. 5
    其他to yield 9.25 g (84%) of a off white solid

实验过程

4-Chloro-pyridine-3-carbaldehyde (10.0 g, 71 mmol) was dissolved in EtOH (12 ml). H2O (30 ml), ice (30 g) and hydroxylamine hydrochloride (5.40 g, 78 mmol) were added. To the resulting mixture was added over a period of 2 min a solution of 2 N NaOH (88.3 ml, 177 mmol). The resulting yellowish solution was stirred 2.5 h at r.t. before neutralisation with AcOH (pH=6). White crystals precipitated, were collected by filtration and washed with H2O (30 ml). The product was dried 1 h at 50° C. on the high vacuum to yield 9.25 g (84%) of a off white solid. m/z=157.1 ([M−H]−).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07825123B2uspto-grants-2010_11