反应 #57299

反应方程式

ethyl chlorothiocarbonate

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

triethylamine

dichloromethane

→

3-(ethylthiocarbonyl)-2-(2-isopropylphenyl)imino-5,5-dimethyl-1,3-thiazine

收率 57.6%

溶剂

water

反应条件

后处理

1. 1
   萃取The mixture was extracted with diethylether (60 ml)
2. 2
   干燥dried over anhydrous magnesium sulfate
3. 3
   浓缩concentrated under reduced pressure
4. 4
   其他The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)

实验过程

To a mixture of 2-(2-isopropylphenyl)imino-5,5-dimethyl-1,3-thiazine (1.00 g), triethylamine (0.58 g) and dichloromethane (5 ml) was added dropwise for 5 minutes ethyl chlorothiocarbonate (0.56 g). The mixture was stirred at room temperature for 1 hour. 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 3-(ethylthiocarbonyl)-2-(2-isopropylphenyl)imino-5,5-dimethyl-1,3-thiazine (0.74 g, yield: 56%) as colorless oil.

来源