反応 #5921

反応方程式

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

収率 165.5%

溶媒

methylene chloride

反応条件

後処理

1. 1
   抽出is extracted with chloroform
2. 2
   洗浄The chloroform layer is washed
3. 3
   その他dried
4. 4
   workup.DISTILLATIONdistilled
5. 5
   その他to remove the solvent
6. 6
   workup.ADDITIONThe residue is treated with hydrochloric acid
7. 7
   その他the resulting salt is recrystallized from ethanol-ether

実験手順

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%).

出典