反应详情

To a solution of 0.9 g (0.0034 Mol) (5-cyclohexyl-2-methoxy-phenyl)-thiourea in 18 ml chloroform were added 0.2 ml (0.0041 Mol) bromine, dissolved in 4.5 ml chloroform and heated to reflux for 16 h. The reaction mixture was diluted with dichloromethane, extracted with sat. aqueous potassium carbonate and brine, dried over sodium sulfate and evaporated to dryness in vacuo. The residue was crystallized from ethyl acetate/diethyl ether to yield 0.61 g (68%) of 7-cyclohexyl-4-methoxy-benzothiazol-2-ylamine as an off-white solid; F.p.: 199-200° C.

1. temperatureheated
2. temperatureto reflux for 16 h
3. extractionextracted with sat. aqueous potassium carbonate and brine
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness in vacuo
6. customThe residue was crystallized from ethyl acetate/diethyl ether