HRID230112

反应详情

EQUATION

反应方程式

HRID 230112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of allylamine (58 mmoles, 3.34 g) at 0° C. in dichloromethane (100 mL) was added triethylamine (120 mmoles, 16 mL). The mixture was stirred for two minutes, then benzylchloroformate (58 mmoles, 8.25 mL) added dropwise. The resulting solution was stirred at 0° C. for 2 hours, and at ambient temperature for an additional 90 minutes. A white precipitate formed, which was filtered off. Solvent was removed from the filtrate under reduced pressure, and the residue chromatographed on a silica gel column, eluting with 20% ethyl acetate/hexanes, to give benzyl allylcarbamate, a compound of formula (2), as a clear oil. Yield: 5.0 g.

WORKUP

后处理

  1. stirringThe resulting solution was stirred at 0° C. for 2 hours
  2. waitat ambient temperature for an additional 90 minutes
  3. customA white precipitate formed
  4. filtrationwhich was filtered off
  5. customSolvent was removed from the filtrate under reduced pressure
  6. customthe residue chromatographed on a silica gel column
  7. washeluting with 20% ethyl acetate/hexanes