반응 #1880

반응 방정식

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

용매

acetone

반응 조건

후처리

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
   농축which was then concentrated under reduced pressure The concentrate
4. 4
   추출was subjected to extraction with ethyl acetate
5. 5
   세척The organic layer was washed with water
6. 6
   기타dried
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

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.

출처