HRID962476

反应详情

EQUATION

反应方程式

HRID 962476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

To methyl 3,5-bis(trifluoromethyl)phenylacetate (43.5 g, 160 mmol), in dry acetonitrile (250 ml), cooled to -5° C., was added 2,4,6-triisopropyl benzenesulfonyl azide (52.7 g). To the resulting solution was added 1,8-diazabicyclo[5.4.0]undec-7-ene (25.5 ml), and the mixture was stirred at -5° C. for 1 hour. The mixture was warmed to room temperature, and then stirred for 0.5 hour. The solvents were evaporated at reduced pressure and the residue purified by chromatography on silica gel (eluant 5% diethyl ether/petroleum ether), to afford the the title compound as yellow prisms. I.R (film, NaCl) 1740, 2140 cm-1.

WORKUP

后处理

  1. temperatureThe mixture was warmed to room temperature
  2. stirringstirred for 0.5 hour
  3. customThe solvents were evaporated at reduced pressure
  4. customthe residue purified by chromatography on silica gel (eluant 5% diethyl ether/petroleum ether)