HRID54714

反应详情

EQUATION

反应方程式

HRID 54714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,2',4,4'-Tetrahydroxybenzophenone (2.5 g, 10.15 mmol.) was heated in 20 ml of water at 195°-200° C. for 4 hours (Aldrich pressure tube). After cooling, the crude product was filtered off and mixed with 25 ml of water. The resulting suspension was refluxed for 25 min. and filtered at about 60° C. Pure product 3,6-dihydroxyxanthone 2.15 g was obtained in 90.4% yield. It did not melt below 330° C. HNMR (DMSO): 10.780 (s,2H), 7.983 (d,2H,J=8.6 Hz), 6,822 (m,4H). MS: 228,220, 1717, 115, 100, 69, 63.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe crude product was filtered off
  3. additionmixed with 25 ml of water
  4. temperatureThe resulting suspension was refluxed for 25 min.
  5. filtrationfiltered at about 60° C