反応 #1880

反応方程式

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

溶媒

acetone

反応条件

後処理

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
   濃縮which was then concentrated under reduced pressure The concentrate
4. 4
   抽出was subjected to extraction with ethyl acetate
5. 5
   洗浄The organic layer was washed with water
6. 6
   その他dried
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

実験手順

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.

出典