反应 #2467926

ord-89c519da4006402697625f65f8045746

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%.

来源

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