反応 #2467926

ord-89c519da4006402697625f65f8045746

反応方程式

C(=NC1CCCCC1)=NC1CCCCC1
Dicyclohexylcarbodiimide
O=C(O)CC(=O)O
Malonic acid
CC(O)c1ccccc1
1-phenyl-ethanol
O=C(NC1CCCCC1)NC1CCCCC1
dicyclohexyl urea

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度with cooling over 10 min so the temperature
  2. 2
    その他did not exceed 30° C

実験手順

Malonic acid (12 g, 0.11 mol) was dissolved in acetonitrile (450 mL) in an Erlenmeyer flask (1 L) together with 1-phenyl-ethanol (26 g, 0.22 mol). Dicyclohexylcarbodiimide (45 g) was added in portions and with cooling over 10 min so the temperature did not exceed 30° C. A precipitate of dicyclohexyl urea formed almost immediately. Stirring at RT continued over the week-end to complete the reaction. Dicyclohexyl urea was removed by filtration and the filter cake was washed with addition acetonitrile (10 mL). The combined solution was evaporated in vacuum to give the crude product as colourless oil. Yield: 29 g, 93%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08257786B2uspto-grants-2012_09