반응 #362092

ord-3b2b6300caa6465698a337d16120f40d

반응 방정식

CCN(CC)CC
Triethylamine
Oc1ccc(Oc2ccccc2)cc1
4-phenoxyphenol
CCCCN=C=O
butyl isocyanate
CCCCNC(=O)Oc1ccc(Oc2ccccc2)cc1
tan solid
수율 99.1%
CCCCNC(=O)Oc1ccc(Oc2ccccc2)cc1
Butylcarbamic acid 4-phenoxyphenyl ester
수율 99.1%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    추출The solution was extracted with 1 N HCl
  3. 3
    건조dried (MgSO4)
  4. 4
    기타the solvent removed under reduced pressure

실험 절차

Triethylamine (15 ml, 0.11 mol) was added dropwise under a nitrogen atmosphere to a solution of 4-phenoxyphenol (25.1 g, 0.14 mol) and butyl isocyanate (18 ml, 0.16 mol) in 400 ml of methylene chloride. After the addition, the solution was stirred overnight at room temperature. The solution was extracted with 1 N HCl, dried (MgSO4) and the solvent removed under reduced pressure to give 39.59 g of a tan solid. Recrystallization from diisopropyl ether gave the title compound as a white crystalline solid (21.01 g, 55%), mp 75°-77° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05391571uspto-grants-1995_02