반응 #5936

반응 방정식

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

수율 108.8%

용매

dichloromethane

dichloromethane

반응 조건

후처리

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

실험 절차

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.

출처