反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooling with an ice-bath
- stirringstirred for 15 hours
- customevaporated
- customThe residue is partitioned between 150 ml methylene chloride and 50 ml of N hydrochloric acid
- customthe organic layer separated
- washwashed with water
- customdried
- filtrationfiltered
- customevaporated
- customThe residue is triturated with diethyl ether
- customrecrystallized from ethanol