반응 #5922

반응 방정식

oxalic acid

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

allyl bromide

potassium carbonate

→

4-(N-allyl-N-methylaminoacetyl)-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine oxalate

용매

water

dimethylformamide

ether

반응 조건

후처리

1. 1
   추출the mixture is extracted with ethyl acetate
2. 2
   workup.DISTILLATIONAfter the solvent is distilled off
3. 3
   기타the residue is purified by silica gel column chromatography (solvent, chloroform:methanol=40:1)
4. 4
   기타The caramel thus obtained
5. 5
   세척The resulting precipitate is washed with ether
6. 6
   기타dried

실험 절차

A mixture of 2-(4-chlorophenyl)-4-(N-methylaminoacetyl)-3,4-dihydro-2H-1,4-benzothiazine (1.80 g), allyl bromide (0.52 ml), potassium carbonate (2.25 g) and dimethylformamide (20 ml) is stirred at room temperature for 3.5 hours. The reaction mixture is poured into water, and the mixture is extracted with ethyl acetate. After the solvent is distilled off, the residue is purified by silica gel column chromatography (solvent, chloroform:methanol=40:1). The caramel thus obtained is dissolved in ether and thereto is added 1.1 equivalent of oxalic acid. The resulting precipitate is washed with ether and dried to give 4-(N-allyl-N-methylaminoacetyl)-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine oxalate as powder.

출처