반응 #5921

반응 방정식

sodium hydrogen carbonate

2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine

N,N-dimethylaniline

dimethylaminoacetyl chloride hydrochloride

→

2-(4-chlorophenyl)-4-(dimethylamino)acetyl-3,4-dihydro-2H-1,4-benzothiazine hydrochloride

수율 165.5%

용매

methylene chloride

반응 조건

후처리

1. 1
   추출is extracted with chloroform
2. 2
   세척The chloroform layer is washed
3. 3
   기타dried
4. 4
   workup.DISTILLATIONdistilled
5. 5
   기타to remove the solvent
6. 6
   workup.ADDITIONThe residue is treated with hydrochloric acid
7. 7
   기타the resulting salt is recrystallized from ethanol-ether

실험 절차

To a solution of 2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine (0.52 g) and N,N-dimethylaniline (0.97 g) in methylene chloride (15 ml) is added dimethylaminoacetyl chloride hydrochloride (0.63 g) under ice cooling, and the mixture is stirred at the same temperature for 2.5 hours. To the reaction mixture is added aqueous sodium hydrogen carbonate solution, and is extracted with chloroform. The chloroform layer is washed, dried and distilled to remove the solvent. The residue is treated with hydrochloric acid and the resulting salt is recrystallized from ethanol-ether to give 2-(4-chlorophenyl)-4-(dimethylamino)acetyl-3,4-dihydro-2H-1,4-benzothiazine hydrochloride (0.63 g, yield 86%).

출처