反应 #1256769
ord-07baa239dfbb4c0dbda1d0ce5446d3e4
反应方程式
4-Chloro-pyridine-3-carbaldehyde
NaOH
H2O
hydroxylamine hydrochloride
→
4-Chloro-pyridine-3-carbaldehyde Oxime
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他White crystals precipitated
- 2过滤were collected by filtration
- 3洗涤washed with H2O (30 ml)
- 4其他The product was dried 1 h at 50° C. on the high vacuum
- 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]−).