HRID463075

反应详情

EQUATION

反应方程式

HRID 463075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

An amount of 2.14 gm (0.005 mol) of 6-[4-(3,4-dichlorophenyl-mercapto)-butoxy]-4,4-dimethyl-4H-3,1-benzoxazin-2-one is dissolved in 50 ml of methanol, mixed with a solution of 1.3 gm (0.06 mol) of sodium metaperiodate in 10 ml of water, and stirred for two hours at ambient temperature. Then, the mixture is refluxed for three hours, the volume of the reaction mixture is reduced by evaporation to about three-quarters, and water is added. The oil precipitated is separated by decanting of the solvent and is taken up in hot isopropanol/disiopropylether. Upon cooling, crystals are obtained which have a melting point of 138°-139° C.

WORKUP

后处理

  1. temperatureThen, the mixture is refluxed for three hours
  2. customthe volume of the reaction mixture is reduced by evaporation to about three-quarters, and water
  3. additionis added
  4. customThe oil precipitated
  5. customis separated
  6. customby decanting of the solvent
  7. temperatureUpon cooling
  8. customcrystals are obtained which