HRID656313

反应详情

EQUATION

反应方程式

HRID 656313 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 2 L flask were added 280.0 g of oxalic acid dihydrate (2.221 moles) and then 1 L of distilled water. Then the mixture was heated to 90° C. After complete dissolution of oxalic acid, 400 mL of concentrated hydrochloric acid was added, followed by addition of 220.0 g of o-phenylenediamine (2.034 moles). The temperature was maintained at 90° C. for 30 minutes with continuous stirring. Off-white crystals were formed. After cooling to room temperature, the off-white crystals were collected by filtration, washed first with water, then with methanol and dried under reduced pressure to give 315.8 g (96%) of off-white needles: mp>350° C.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe temperature was maintained at 90° C. for 30 minutes with continuous stirring
  3. customOff-white crystals were formed
  4. temperatureAfter cooling to room temperature
  5. filtrationthe off-white crystals were collected by filtration
  6. washwashed first with water
  7. dry with materialwith methanol and dried under reduced pressure