HRID543082

反应详情

EQUATION

反应方程式

HRID 543082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitto deposit within a few minutes
  2. customPrecipitation
  3. additionwas completed by addition of diethyl ether
  4. filtrationThe product was collected by filtration
  5. customto give 5.5 g, 86.5% of theory, m.p. 210°-234° C
  6. customThe product was recrystallized