반응 #2467926

ord-89c519da4006402697625f65f8045746

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도with cooling over 10 min so the temperature
  2. 2
    기타did not exceed 30° C

실험 절차

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%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08257786B2uspto-grants-2012_09