反应 #5936

反应方程式

chloroacetyl chloride

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

triethylamine

→

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

收率 108.8%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   workup.DISTILLATIONAfter the solvent is distilled off, to the residue
2. 2
   workup.ADDITIONare added ethyl acetate and water
3. 3
   洗涤the ethyl acetate layer is washed with aqueous sodium hydrogen carbonate solution, water and saline
4. 4
   干燥dried over sodium sulfate
5. 5
   workup.DISTILLATIONdistilled
6. 6
   其他to remove the solvent

实验过程

To a suspension of (R)-(+)-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine (1.30 g, 0.005 mole) and triethylamine (1.66 ml, 0.012 mole) in dichloromethane (16 ml) is added dropwise a solution of chloroacetyl chloride (0.79 ml, 0.01 mole) in dichloromethane (4 ml) under ice cooling, and the mixture is stirred at room temperature for 45 minutes. After the solvent is distilled off, to the residue are added ethyl acetate and water, and the ethyl acetate layer is washed with aqueous sodium hydrogen carbonate solution, water and saline, dried over sodium sulfate and distilled to remove the solvent to give (R)-4-chloroacetyl-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine (1.84 g) as caramel.

来源