Hydroxyamine hydrochloride → HCID 178471847, Verbindung

HRID 2189781Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2189781
[C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]=[CH:6]2)#[N:2].C(=O)(O)[O-].[Na+].Cl.[NH2:25][OH:26]>C(O)C>[OH:26][NH:25][C:1](=[NH:2])[C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]=[CH:6]2

Komponenten

5

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 59316705Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate

Produkt 1

HCID 178471847HCID 178471847, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate (D47) (3.84 g, 15.8 mmol) was dissolved in ethanol (100 ml) and sodium bicarbonate (6.6 g, 79 mmol) and then hydroxylamine hydrochloride (3.3 g, 47.4 mmol) were added. The reaction was heated to 50° C. for a total of 11 hours and then left to cool overnight. The reaction was filtered and the residue washed with ethanol. The filtrate was evaporated to dryness in vacuo and the resultant solid triturated with ether to generate the title compound (3.79 g) as a white solid. MS (ES): C13H16N4O3 requires 276; found (MH+) 277.

Aufarbeitung

  1. waitleft
  2. temperatureto cool overnight
  3. filtrationThe reaction was filtered
  4. washthe residue washed with ethanol
  5. customThe filtrate was evaporated to dryness in vacuo
  6. customthe resultant solid triturated with ether

Quellen und Nachweise

ORD-Eintrag
ord-799d95a2309f4ed4acc65eada05d0b08
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08324254B2

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