반응 #442504

ord-ae8ddf0e4bbe40c6be64f22f15a190ee

반응 방정식

C=CCCCCCCCCO
9-Decen-1-ol
O=C1C=CC(=O)O1
maleic anhydride
Cc1ccc(S(=O)(=O)O)cc1
p-toluenesulfonic acid
Cc1ccccc1
toluene
C=CCCCCCCCCOC(=O)/C=C\C(=O)OCCCCCCCCC=C
Di(9-decen-1-yl) Maleate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타fitted with a condenser
  2. 2
    온도The mixture was heated
  3. 3
    온도to reflux for 18 h
  4. 4
    농축The cooled mixture was concentrated by rotary evaporation
  5. 5
    workup.DISTILLATIONstripped by Kugelrohr distillation
  6. 6
    기타to remove excess alcohol

실험 절차

9-Decen-1-ol (Rosalva) in the amount of 50.00 g (0.320 mol) and maleic anhydride in the amount of 12.55 g (0.128 mol), toluene in the amount of 200 ml, and p-toluenesulfonic acid in the amount of 1.24 g (6.40 mmol) were combined in a flask fitted with a condenser, Dean-Stark trap, and argon inlet. The mixture was heated to reflux for 18 h. The cooled mixture was concentrated by rotary evaporation and then stripped by Kugelrohr distillation to remove excess alcohol. Purity of the product was determined by thin layer chromatography and the structure confirmed by 1H and 13C NMR.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05830835uspto-grants-1998_11