HRID1444661

反应详情

EQUATION

反应方程式

HRID 1444661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Dimethyl sulfate (22.84 mL, 240 mmol) and dimethyl trithiocarbonate (26.48 mL, 240 mmol) were added to acetonitrile (80 mL). The resultant dark yellow solution was heated to 90° C. for 2 hours. The mixture was then allowed to cool to 55° C. and then a solution of tetrafluoroboric acid (54% in diethyl ether, 48 mL) was added over 5 min time. The resultant solution was stirred for an additional 15 min, followed by pouring it into a solution of ice-cold diethyl ether (600 mL), The white solid that formed was collected and washed with diethyl ether (3×50 mL) and dried in a vacuum oven to provide (bis-methylsulfanyl -methylene)-methyl-sulfonium tetrafluoroborate salt (47.3 g, 83%) as a colorless solid.

WORKUP

后处理

  1. temperatureto cool to 55° C.
  2. customThe white solid that formed
  3. customwas collected
  4. washwashed with diethyl ether (3×50 mL)
  5. customdried in a vacuum oven