反应 #1328418
ord-0dfed2e448b741f088cef3ac6046a011
反应方程式
sulfuric acid
8-methylthio-3a,4-dihydro-3H-indeno[1,2-c]isoxazole
bromine
→
5-Bromo-8-methylthio-3a,4-dihydro-3H-indeno[1,2-c]isoxazole
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.STIRRINGthis mixture was stirred for 1.5 hours
- 2过滤the precipitated solid was filtered off with suction
- 3洗涤washed
- 4其他dried
实验过程
120 ml of sulfuric acid (98 percent strength) were cooled to 0° C., and 11.2 g (54.8 mmol) of 8-methylthio-3a,4-dihydro-3H-indeno[1,2-c]isoxazole were added a little at a time. 9.2 g (57.5 mmol) of bromine were then added dropwise, and stirring was continued at 0° C. for another 2 hours. The resulting solution was poured into 2 l of a mixture of water and ice, this mixture was stirred for 1.5 hours and the precipitated solid was filtered off with suction and then washed and dried. This gave 11.4 g (73%) of 5-bromo-8-methylthio-3a,4-dihydro-3H-indeno[1,2-c]isoxazole of a brown solid having a m.p. of 127–135° C.