反应详情

To a stirred solution of 2-(3-nitro-phenyl)-thiazole (18.5 g, 89.7 mmol) in a mixture of chloroform (150 ml) and anhydrous DMF (40 ml) was slowly added sulfuryl chloride (28.2 ml, 359 mmol). After the addition, the resultant mixture was stirred at reflux for 3 hours. The cooled mixture was concentrated under reduced pressure and the residue was partitioned between aqueous calcium chloride (3M) and ethyl acetate. The organic layer was washed with aqueous sodium carbonate, dried over magnesium sulphate and evaporated to dryness to leave the desired product. 20.6 g (80%).

1. additionAfter the addition
2. temperatureat reflux for 3 hours
3. concentrationThe cooled mixture was concentrated under reduced pressure
4. customthe residue was partitioned between aqueous calcium chloride (3M) and ethyl acetate
5. washThe organic layer was washed with aqueous sodium carbonate
6. dry with materialdried over magnesium sulphate
7. customevaporated to dryness