HRID267767

反应详情

EQUATION

反应方程式

HRID 267767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 4.92 g. (30 millimoles) of 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin in 100 mls. of benzene is added dropwise a solution of 30 millimoles of anhydrous hydrogen cyanide in 50 ml. of benzene. The reaction mixture is stirred overnight at ambient temperature, basified with 10% sodium carbonate solution and the organic layer separated. The benzene solution is washed once with water and dried successively over anhydrous magnesium sulfate and calcium sulfate. Evaporation of the solvent under reduced pressure at 40° C. yields the crude cyanohydrin which upon purification and mixed melting point determination gives no depression with an authentic sample of 3-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin.

WORKUP

后处理

  1. customthe organic layer separated
  2. washThe benzene solution is washed once with water
  3. dry with materialdried successively over anhydrous magnesium sulfate and calcium sulfate
  4. customEvaporation of the solvent under reduced pressure at 40° C.
  5. customyields the crude cyanohydrin which
  6. customupon purification
  7. additionmixed