4,4-Dimethylpyrrolidine-2-carboxylic acid → 4,4-Dimethyl-1-nitrosopyrrolidine-2-carboxylic acid

HRID 2216600Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2216600
[CH3:1][C:2]1([CH3:10])[CH2:6][NH:5][CH:4]([C:7]([OH:9])=[O:8])[CH2:3]1.[N:11]([O-])=[O:12].[Na+]>CC(O)=O.O>[CH3:1][C:2]1([CH3:10])[CH2:6][N:5]([N:11]=[O:12])[CH:4]([C:7]([OH:9])=[O:8])[CH2:3]1

Komponenten

5

Edukt 2

HCID 2866424,4-Dimethylpyrrolidine-2-carboxylic acidHCID 23668193Sodium Nitrite

Produkt 1

HCID 219413404,4-Dimethyl-1-nitrosopyrrolidine-2-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a suspension of 37.5 g of the crude 4,4-dimethylpyrrolidine-2-carboxylic acid in 420 mL of AcOH was added a solution of 13.3 g (0.19 mol) of NaNO2 in 210 mL of water over 15 min at room temperature and stirred for 3 h. The solution was concentrated under reduced pressure. Acetone (250 mL) was added to the residue and the precipitate was filtered off, and the solution was concentrated under reduced pressure to dryness and crude 4,4-dimethyl-1-nitrosopyrrolidine-2-carboxylic acid was obtained as brown oil.

Aufarbeitung

  1. concentrationThe solution was concentrated under reduced pressure
  2. additionAcetone (250 mL) was added to the residue
  3. filtrationthe precipitate was filtered off
  4. concentrationthe solution was concentrated under reduced pressure to dryness

Quellen und Nachweise

ORD-Eintrag
ord-8ef930529d904727ba5f66acf342bd45
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07112582B2

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