HRID372790

反应详情

EQUATION

反应方程式

HRID 372790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 19.3 g of N-benzyl-N-chloroacetyl-3-hydroxy-3,3-diphenylpropylamine in 150 ml of dimethylformamide is added dropwise to the suspension of 1.2 g of sodium hydride in 50 ml of dimethylformamide while stirring and cooling with an ice-bath. The mixture is allowed to warm up to room temperature, stirred for 15 hours and evaporated. The residue is partitioned between 150 ml methylene chloride and 50 ml of N hydrochloric acid, the organic layer separated, washed with water, dried, filtered and evaporated. The residue is triturated with diethyl ether and recrystallized from ethanol, to yield the 4-benzyl-3-oxo-7,7-diphenyl-hexahydro-1,4-oxazepine of the formula ##STR7## melting at 185° to 186°.

WORKUP

后处理

  1. temperaturecooling with an ice-bath
  2. stirringstirred for 15 hours
  3. customevaporated
  4. customThe residue is partitioned between 150 ml methylene chloride and 50 ml of N hydrochloric acid
  5. customthe organic layer separated
  6. washwashed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue is triturated with diethyl ether
  11. customrecrystallized from ethanol