Hydroxylamine → HCID 178526327, Verbindung

HRID 464646Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 464646
[NH2:1][OH:2].Cl.NO.C(=O)([O-])[O-].[Na+].[Na+].S([C:22]1[CH:27]2[CH2:28][CH:24]([CH:25]=[CH:26]2)[N:23]=1)(C1C=CC(C)=CC=1)(=O)=O>O1CCCC1>[CH:24]12[CH2:28][CH:27]([CH:26]=[CH:25]1)[C:22](=[N:1][OH:2])[NH:23]2

Komponenten

6

Edukt 4

HCID 787HydroxylamineHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 21998189HCID 21998189, Verbindung

Produkt 1

HCID 178526327HCID 178526327, VerbindungAusbeute 30,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

To a solution of hydroxylamine (from 2.1 g (0.03 m) of hydroxylamine hydrochloride, 4.3 g (0.015 m) of sodium carbonate, 10 ml of water and 200 ml of tetrahydrofuran) at 0° C. was added 5.16 g (0.021 m) of 3-tosyl-2-azabicyclo[2.2.1]hepta-2,5-diene (prepared by the procedure of J. Organic Chemistry, 39, 564 (1974)) in 50 ml of tetrahydrofuran. After being stirred overnight, during which time the temperature was allowed to warm to 25° C., the organic layer was separated, dried, and stripped of solvent. Purification of the residue by chromatography (silica gel: 1:1::dichloromethane:ethyl acetate) gave 0.8 g of material whose spectra were consistent with the title structure.

Aufarbeitung

  1. customprepared by the procedure of J
  2. customthe organic layer was separated
  3. customdried
  4. customPurification of the residue by chromatography (silica gel: 1:1::dichloromethane:ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-ddf96b98a2af4e469092a249ac9243f2
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548929

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