HRID60624
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
4-Fluoro-3-nitrobenzyl alcohol (3.17 g, 18.5 mmol) was suspended in EtOH, and a slurry of palladium on carbon (10 wt %, 317 mg) in EtOH was added. The flask was sealed with a septum, evacuated, and a H2 filled balloon was introduced via syringe and the reaction was stirred at RT overnight. The reaction mixture was then filtered through a pad of Celite, washed with EtOH and the filtrates concentrated in vacuo to afford a oil which upon scratching crystallised to give the title compound (2.56 g, 98%). 1H NMR (300 MHz, CDCl3): 4.57 (2H, s), 6.63-6.71 (1H, m), 6.77-6.84 (1H, m), 6.90-7.00 (1H, dd, J=8.2, 11.0 Hz). No OH or NH signals observed.
WORKUP
后处理
- customThe flask was sealed with a septum
- customevacuated
- additiona H2 filled balloon was introduced via syringe
- filtrationThe reaction mixture was then filtered through a pad of Celite
- washwashed with EtOH
- concentrationthe filtrates concentrated in vacuo
- customto afford a oil which
- customupon scratching crystallised