HRID922294
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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To a 250 mL RB flask fitted with magnetic stirrer was charged with hydroxylamine hydrochloride (5 g, 73 mmol) in water, then slowly added 50% of NaOH solution. To this stirred solution, added phthalic anhydride (11.26 g, 76 mmol), stirred at 90° C. for 40 min. Then cooled to RT, yellowish solid was removed by filtration. The filtrate was neutralized with 30% of H2SO4 and solid was precipitated. The solid was filtered off on Buchner flask and dried under line vacuum to obtain the title compound (6.5 g, Yield: 55.34%): 1H NMR (300 MHz, DMSO-d6): δ 10.80 (s, 1H), 7.84 (s, 4H).
WORKUP
后处理
- customTo a 250 mL RB flask fitted with magnetic stirrer
- temperatureThen cooled to RT
- customyellowish solid was removed by filtration
- customwas precipitated
- filtrationThe solid was filtered off on Buchner flask
- customdried under line vacuum