反应详情

2-Methylbenzotellurazole (Example 18) (10.5 g, 0.043 mole) was dissolved in dry dichloromethane (75 ml). Freshly distilled methyl trifluoromethanesulfonate (7.5 g, 0.045 mole) was added to the solution. An exothermic reaction occurred immediately. After a few minutes a crystalline product separated which was collected by filtration, washed with diethyl ether, and dried. Yield 16.86 g (96%). The pale yellow powder was dissolved in acetone (100 ml) and reprecipitated by adding diethyl ether to the solution until it became turbid. Colorless plates separated on chilling. Yield 15.33 g (87% of theory); mp 160°-162° C.

1. customAn exothermic reaction
2. customAfter a few minutes a crystalline product separated which
3. filtrationwas collected by filtration
4. washwashed with diethyl ether
5. customdried
6. dissolutionThe pale yellow powder was dissolved in acetone (100 ml)
7. customreprecipitated
8. additionby adding diethyl ether to the solution until it
9. customColorless plates separated
10. temperatureon chilling