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1,1'-Carbonyldiimidazole → HCID 69662350, Verbindung

HRID 857188
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 857188
[C:1]([O:4][CH2:5][C:6]([OH:9])([CH3:8])[CH3:7])(=[O:3])[CH3:2].[C:10](N1C=CN=C1)([N:12]1[CH:16]=[CH:15][N:14]=[CH:13]1)=[O:11]>C(Cl)Cl>[N:12]1([C:10]([O:9][C:6]([CH3:8])([CH3:7])[CH2:5][O:4][C:1](=[O:3])[CH3:2])=[O:11])[CH:16]=[CH:15][N:14]=[CH:13]1
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Komponenten

4

Edukt 2

HCID 682631,1'-CarbonyldiimidazoleHCID 110839221,2-Propanediol, 2-methyl-, 1-acetate

Produkt 1

HCID 69662350HCID 69662350, VerbindungAusbeute 20 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 2-hydroxy-2-methylpropyl acetate (3.35 g, 25.3 mmol) and 1,1′-carbonyldiimidazole (4.11 g, 25.3 mmol) in DCM was stirred for 8 h at rt. The mixture was then transferred to a closed vessel and heated to 100° C. overnight. The mixture was concentrated in vacuo before ether and water were added. The organic phase was separated, dried and concentrated in vacuo. The resulting residue was purified by chromatography on silica gel, eluting with THF:heptane (1:1), to give the title compound in 20% yield.

Aufarbeitung

  1. customThe mixture was then transferred to a closed vessel
  2. temperatureheated to 100° C. overnight
  3. concentrationThe mixture was concentrated in vacuo before ether and water
  4. additionwere added
  5. customThe organic phase was separated
  6. customdried
  7. concentrationconcentrated in vacuo
  8. customThe resulting residue was purified by chromatography on silica gel
  9. washeluting with THF:heptane (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-d1c66f5f4c4545aa97dfd233f1fa1167
Quelldatensatz
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07144914B2

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