Oxalic Acid → HCID 9837977, Verbindung

HRID 1655102Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1655102
[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[CH3:7][C:8]1[CH:12]=[C:11]([CH:13]2[CH2:17][CH2:16][CH2:15][N:14]2[CH3:18])[O:10][N:9]=1>C(OCC)C>[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[CH3:7][C:8]1[CH:12]=[C:11]([C@@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[CH3:18])[O:10][N:9]=1

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 15186066HCID 15186066, Verbindung

Produkt 1

HCID 9837977HCID 9837977, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of oxalic acid (51 mg, 0.57 mmol) in diethyl ether was added dropwise to a stirring solution of 3-methyl-5-(1-methyl-2-pyrrolidinyl)-isoxazole (62.8 mg, 0.38 mmol), from Example 2a, in diethyl ether. After 0.5 hour of stirring at ambient temperature, the reaction flask became coated with a glass-like clear colorless solid. The diethyl ether was evaporated and the solid was triturated several times with diethyl ether to give, after evaporation of the solvent in vacuo, 102 mg of the title compound (2b). MS (DCl/NH3) m/e 167 (M+H)+, 184 (M+NH4)+. 1H NMR (D2O) δ: 2.11-2.33 (m, 3H), 2.31 (s, 3H), 2.49-2.60 (m, 1H), 2.48 (dd, 2H), 4.92 (t, 1H), 6.52 (s, 1H). Anal. calcd. for C10H13NO5.0.2H2O.0.2C2H2O 2 : C, 48.65; H, 6.16; N, 9.95. Found: C, 48.80; H, 5.90; N, 9.77.

Aufarbeitung

  1. customThe diethyl ether was evaporated
  2. customthe solid was triturated several times with diethyl ether
  3. customto give
  4. customafter evaporation of the solvent in vacuo, 102 mg of the title compound (2b)

Quellen und Nachweise

ORD-Eintrag
ord-31aa152bd6c544f7a48204873742d315
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05409946

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