HRID1414175

反应详情

EQUATION

反应方程式

HRID 1414175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Hydroxy-1,2-bis(3-hydroxyphenyl)ethanone was reduced by the procedure of M. Pisova and M. Soncek [Coll. Czech, Chem. Comm., 38, 3876 (1973)]. A mixture of 2-hydroxy-1,2-bis(3-hydroxyphenylethanone (18 g.) chromic sulfate hydrate (20.9% Cr; 60 g.), zinc dust (49 g.) and water-ethanol (1:1, 1 liter) was stirred under an atmosphere of nitrogen for 11 hours. The mixture was diluted with water and extracted with three portions of ethyl acetate. The organic solution was washed with saturated brine solution and dried over magnesium sulfate. The solution was concentrated and the product crystallized from ethyl acetate-benzene (seeding); yield: 8.51 g., m.p. 155°-156°.

WORKUP

后处理

  1. extractionextracted with three portions of ethyl acetate
  2. washThe organic solution was washed with saturated brine solution
  3. dry with materialdried over magnesium sulfate
  4. concentrationThe solution was concentrated
  5. customthe product crystallized from ethyl acetate-benzene (seeding)