HRID1258150

反应详情

EQUATION

反应方程式

HRID 1258150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of piperidin-4-ylcarbamic acid tert-butyl ester (2.5 g, 12.4 mmol), 3,4,5-trifluorobenzyl bromide (2.5 g, 11.3 mmol) and diisoproylethylamine (2.9 ml, 16.9 mmol) in dichloromethane (25 ml) was stirred at room temperature for 2 h. After this period, trifluoroacetic acid (15.6 ml) was added and the reaction was stirred for a further 2 h. The solvent was evaporated in vacuo and a saturated solution of sodium carbonate was added. The mixture was extracted with dichloromethane and the separated organic layers were dried (Na2SO4), filtered, and the solvent evaporated in vacuo to yield D8 (2.9 g, 96%) as a solid. C12H15F3N2 requires 244. Found 245 (MH+)

WORKUP

后处理

  1. waitAfter this period
  2. stirringthe reaction was stirred for a further 2 h
  3. customThe solvent was evaporated in vacuo
  4. additiona saturated solution of sodium carbonate was added
  5. extractionThe mixture was extracted with dichloromethane
  6. dry with materialthe separated organic layers were dried (Na2SO4)
  7. filtrationfiltered
  8. customthe solvent evaporated in vacuo