HRID581647

反应详情

EQUATION

反应方程式

HRID 581647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of thioxanthone (10 g) in 60 mL of benzene was treated with 5.0 g of LAH by stirring for 15 min. The mixture was heated and 100 mL of ether was added carefully. Reflux was continued for 90 min. The cooled mixture was neutralized with water. The solids were filtered off and the filtrate evaporated to dryness. Pure thioxanthene (9.1 g, 98%) was isolated by chromatography using 20% ethyl acetate/hexane; 1H NMR (CDCl3) δ 3.82 (s, 3H), 7.21 (m, 4H), 7.33 (m, 2H), 7.46 (m, 2H).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureReflux
  3. waitwas continued for 90 min
  4. filtrationThe solids were filtered off
  5. customthe filtrate evaporated to dryness