反应详情

温度

60 °C

0.966 g of 2-amino-4-chloro-benzenethiol was dissolved in 10 ml of abs. ethanol. 1.44 g of 2-chloro-1,1,1-triethoxy-ethane were added and the reaction was heated at 60° C. overnight. The reaction mixture was then concentrated in vacuo, dissolved in diethyl ether and the organic phase was washed once each with 5% aqueous hydrochloric acid, followed by water and 10% aqueous sodium bicarbonate. The organic layer was dried with magnesium sulfate and concentrated in vacuo. Purification by flash chromatography on silica with heptanes/dichloromethane afforded 1.071 g of 5-chloro-2-chloromethyl benzothiazole as a yellow solid.

1. concentrationThe reaction mixture was then concentrated in vacuo
2. dissolutiondissolved in diethyl ether
3. washthe organic phase was washed once each with 5% aqueous hydrochloric acid
4. dry with materialThe organic layer was dried with magnesium sulfate
5. concentrationconcentrated in vacuo
6. customPurification by flash chromatography on silica with heptanes/dichloromethane