반응 #57305

반응 방정식

ethyl chlorothiocarbonate

2-(2-methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine

triethylamine

dichloromethane

→

2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine

수율 60.0%

용매

water

반응 조건

후처리

1. 1
   추출The mixture was extracted with diethylether (60 ml)
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   농축concentrated under reduced pressure
4. 4
   기타The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)

실험 절차

To a mixture of 2-(2-methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine (0.28 g), triethylamine (0.15 g) and dichloromethane (5 ml) was added dropwise for 3 minutes ethyl chlorothiocarbonate (0.15 g). The mixture was stirred at room temperature for 2 hours. To the solution was added water (30 ml). The mixture was extracted with diethylether (60 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to give 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine (0.21 g, yield: 60%) as colorless oil.

출처