HRID1008266

反应详情

EQUATION

反应方程式

HRID 1008266 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

In a 1000-ml three-neck flask equipped with a thermometer, a reflux condenser and a stirrer were placed 50 g of o-xylylene oxide, 87.5 g of 60% by weight nitric acid, 163.8 g of water, and 198.8 g of acetic acid. The mixture was raised in temperature to 70° C. on an oil bath and was stirred under these conditions for 1 hour. After cooling, the reaction mixture was analyzed by gas chromatography to find that the raw material o-xylylene oxide was completely absent and that phthalaldehyde was formed in a yield of 86%. Phthalide was formed in a yield of 13% as a by-product. The obtained reaction mixture was extracted with two portions of toluene, the organic layer was distilled and thereby yielded phthalaldehyde in a yield of 70% on the basis of o-xylylene glycol. Gas chromatographic analysis revealed that phthalaldehyde had a purity of 99.0%.

WORKUP

后处理

  1. customIn a 1000-ml three-neck flask equipped with a thermometer, a reflux condenser and a stirrer
  2. temperatureAfter cooling