HRID543082
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5,6-Dimethoxy-2-methylbenzotellurazole (Example 19) (4.8 g=0.013 mole) was dissolved in dichloromethane (75 ml), and methyl trifluoromethanesulfonate (2.48 g=1.66 ml=0.013 mole) was added. The solution turned cloudy and crystals started to deposit within a few minutes. Precipitation was completed by addition of diethyl ether. The product was collected by filtration to give 5.5 g, 86.5% of theory, m.p. 210°-234° C. The product was recrystallized from boiling acetone (≃130 ml required) m.p. 242°-243° C.
WORKUP
后处理
- waitto deposit within a few minutes
- customPrecipitation
- additionwas completed by addition of diethyl ether
- filtrationThe product was collected by filtration
- customto give 5.5 g, 86.5% of theory, m.p. 210°-234° C
- customThe product was recrystallized