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Ethanol → HCID 13656010, Verbindung

HRID 745899
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 745899
[CH3:1][Si:2]([CH3:12])([CH3:11])[C:3]#[C:4][CH2:5][CH2:6][CH2:7][C:8]([OH:10])=[O:9].[CH2:13](O)[CH3:14].N1C=CC=CC=1>O1CCCC1>[CH3:12][Si:2]([CH3:1])([CH3:11])[C:3]#[C:4][CH2:5][CH2:6][CH2:7][C:8]([O:10][CH2:13][CH3:14])=[O:9]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 702EthanolHCID 1049PyridineHCID 119900745-Hexynoic acid, 6-(trimethylsilyl)-

Produkt 1

HCID 13656010HCID 13656010, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of 5.3 gm of 1,1-carbonyldiimidazole in 80 ml of dry tetrahydrofuran under argon, was added a solution of 5.03 gm of 6-trimethylsilyl-5-hexynoic acid in 15 ml of dry tetrahydrofuran. The mixture was stirred for 1 hour. Absolute ethanol (80 ml) and pyridine (1 ml) were then added, and the resulting mixture was stirred at room temperature for 48 hours. The solvent was evaporated and the residual oil was extracted with ether and 1.5% hydrochloric acid. The ethereal layer, which was washed with water and then dried, was evaporated to an oil. This material was purified by distillation, b.p. 70°-75° C. (0.6 mm Hg); IR: 2170, 1735 cm-1.

Aufarbeitung

  1. stirringthe resulting mixture was stirred at room temperature for 48 hours
  2. customThe solvent was evaporated
  3. extractionthe residual oil was extracted with ether and 1.5% hydrochloric acid
  4. washThe ethereal layer, which was washed with water
  5. customdried
  6. customwas evaporated to an oil
  7. distillationThis material was purified by distillation, b.p. 70°-75° C. (0.6 mm Hg)

Quellen und Nachweise

ORD-Eintrag
ord-83430d2080774b3f8ba143fafc677b13
Quelldatensatz
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04602006

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