Sulfuric acid magnesium salt (1:1) → HCID 178480450, Verbindung

HRID 624297Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 624297
[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH:8]=O)[CH:3]=1.[NH2:10][CH:11]1[CH2:15][CH2:14][N:13]([CH3:16])[C:12]1=[O:17].S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4](/[CH:8]=[N:10]/[CH:11]2[CH2:15][CH2:14][N:13]([CH3:16])[C:12]2=[O:17])[CH:3]=1

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 147614724-Bromopyridine-2-carbaldehydeHCID 457911333-Amino-1-methylpyrrolidin-2-one

Produkt 1

HCID 178480450HCID 178480450, VerbindungAusbeute 93,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a stirred solution of 4-bromopyridine-2-carbaldehyde (2232.1 mg, 12 mmol) in anhydrous DCM (60 mL) under nitrogen at room temperature, was added racemic 3-amino-1-methyl-pyrrolidin-2-one (1506.8 mg, 13.2 mmol) [CAS: 2483-65-0] and magnesium sulfate (4500 mg, 37.4 mmol). The resulting mixture was left to stir at room temperature overnight. It was filtered and the filtrate washed with half saturated brine. The organic layer was dried (Na2SO4) and evaporated to give 3-[(E)-(4-bromo-2-pyridyl)methyleneamino]-1-methyl-pyrrolidin-2-one (D1) (3.15 g, 11.2 mmol, 93% yield), as a cream solid;

Aufarbeitung

  1. waitThe resulting mixture was left
  2. filtrationIt was filtered
  3. washthe filtrate washed with half saturated brine
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-ea285e6bbc5541afb82dcacc26b4c143
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09303032B2

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