HRID71704

反应详情

EQUATION

反应方程式

HRID 71704 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

The suspension of (4,4′-dibromo-2′-hydroxymethyl-biphenyl-2-yl)-methanol (460 mg) in phosphoric acid (25 ml) was heated at 160° C. for 4 hours. The mixture was cooled and diluted with water (100 ml), and was extracted with EtOAC. The organic phase was washed with water, saturated sodium bicarbonate, and brine, and was dried with sodium sulfate. Concentration yielded 3,9-dibromo-5,7-dihydro-dibenzo[c,e]oxepine (416 mg).

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. extractionwas extracted with EtOAC
  3. washThe organic phase was washed with water, saturated sodium bicarbonate, and brine
  4. dry with materialwas dried with sodium sulfate
  5. concentrationConcentration