Triethylamine → HCID 53975722, Verbindung

HRID 1090885Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1090885
[CH2:1]([N:13]=[C:14]=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].N[CH2:17][C:18]1[CH:19]=[C:20]([Si:23]([CH2:28][CH3:29])([CH2:26][CH3:27])[CH2:24][CH3:25])[O:21][CH:22]=1.C([N:32](CC)CC)C>O1CCCC1>[CH2:1]([N:13]([CH2:17][C:18]1[CH:19]=[C:20]([Si:23]([CH2:24][CH3:25])([CH2:28][CH3:29])[CH2:26][CH3:27])[O:21][CH:22]=1)[C:14]([NH2:32])=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 77873Dodecane, 1-isocyanato-HCID 150370494-Aminomethyl-2-triethylsilylfuran2×

Produkt 1

HCID 53975722HCID 53975722, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Dodecylisocyanate (105 mg, 0.49 mmol) was added to a solution of 4-aminomethyl-2-triethylsilylfuran (Compound 2, 70 mg, 0.33 mmol) and triethylamine (69 microliter, 0.49 mmol) in tetrahydrofuran (3 ml) at room temperature. After stirring at room temperature overnight (ca. 16 hours), the reaction mixture was quenched with water. Extraction (ethyl ether) and evaporation of the dried (magnesium sulfate) extracts gave a residue which was purified by flash chromatography on silica using 60% ethyl ether/hexane. Fractions of Rf of about 0.47 on evaporation gave the title urea as an off-white solid.

Aufarbeitung

  1. customthe reaction mixture was quenched with water
  2. extractionExtraction (ethyl ether) and evaporation of the
  3. dry with materialdried (magnesium sulfate)
  4. customextracts gave a residue which
  5. customwas purified by flash chromatography on silica using 60% ethyl ether/hexane
  6. customFractions of Rf of about 0.47 on evaporation

Quellen und Nachweise

ORD-Eintrag
ord-e5ab4637f585402494b2fac6f86aa150
Quelldatensatz
uspto-grants-1992_01
Patentnummer
US05082954

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