反応 #5922

反応方程式

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

溶媒

water

dimethylformamide

ether

反応条件

後処理

1. 1
   抽出the mixture is extracted with ethyl acetate
2. 2
   workup.DISTILLATIONAfter the solvent is distilled off
3. 3
   その他the residue is purified by silica gel column chromatography (solvent, chloroform:methanol=40:1)
4. 4
   その他The caramel thus obtained
5. 5
   洗浄The resulting precipitate is washed with ether
6. 6
   その他dried

実験手順

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.

出典