Formaldehyde → HCID 67981250, Verbindung

HRID 1520026Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1520026
[CH2:1]=O.Cl.[N+:4]([C:7]1[CH:8]=[N:9][N:10]([CH:12]2[CH2:16][CH2:15][NH:14][CH2:13]2)[CH:11]=1)([O-:6])=[O:5]>C(O)=O>[CH3:1][N:14]1[CH2:15][CH2:16][CH:12]([N:10]2[CH:11]=[C:7]([N+:4]([O-:6])=[O:5])[CH:8]=[N:9]2)[CH2:13]1

Komponenten

4

Edukt 2

HCID 712FormaldehydeHCID 67981150HCID 67981150, Verbindung

Produkt 1

HCID 67981250HCID 67981250, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 284Formic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of Formic acid (50 ml) and Formaldehyde solution (50 mL) was added 4-Nitro-1-pyrrolidin-3-yl-1H-pyrazole hydrochloride (10 g). The reaction mixture was heated at 100° C. for 16 h. The reaction mixture was concentrated under reduced pressure. The residue was tarturated with acetonitrile (150 mL), filtered off solid and filtrate was concentrated. The crude material was basified with ammonia solution, extracted with ethyl acetate, dried over sodium sulphate and evaporated to afford (7 g, 78%) as pale yellow liquid. 1H NMR (400 Mz, DMSO-d6) δ 8.85 (s, 1H), 8.24 (s, 1H), 5.24 (m, 1H), 2.75-2.81 (m, 3H), 2.33-2.49 (m, 2H), 2.27 (s, 3H), 2.12 (m, 1H).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. filtrationfiltered off solid and filtrate
  3. concentrationwas concentrated
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over sodium sulphate
  6. customevaporated
  7. customto afford (7 g, 78%) as pale yellow liquid

Quellen und Nachweise

ORD-Eintrag
ord-a2fa40ec113641f986fb3ef5877c1fac
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073892B2

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