HRID922294

反应详情

EQUATION

反应方程式

HRID 922294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customTo a 250 mL RB flask fitted with magnetic stirrer
  2. temperatureThen cooled to RT
  3. customyellowish solid was removed by filtration
  4. customwas precipitated
  5. filtrationThe solid was filtered off on Buchner flask
  6. customdried under line vacuum