反应 #1880

反应方程式

trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-methanol

Jones reagent

→

trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-carboxylic acid

溶剂

acetone

反应条件

后处理

1. 1
   workup.ADDITIONTo the solution was added dropwise
2. 2
   workup.STIRRINGThe reaction mixture was stirred for one hour at room temperature
3. 3
   浓缩which was then concentrated under reduced pressure The concentrate
4. 4
   萃取was subjected to extraction with ethyl acetate
5. 5
   洗涤The organic layer was washed with water
6. 6
   其他dried
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

实验过程

In 20 ml of acetone was dissolved 0.5 g of trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-methanol obtained in Example 46. To the solution was added dropwise, while stirring at room temperature, 0.5 ml of a Jones reagent. The reaction mixture was stirred for one hour at room temperature, which was then concentrated under reduced pressure The concentrate was subjected to extraction with ethyl acetate. The organic layer was washed with water and dried, then the solvent was distilled off under reduced pressure. From the residue was obtained 0.23 g of trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-carboxylic acid as white crystals, m.p.177°-178 C.

来源