Sodium Hydroxide → N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

HRID 866302Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 866302
[BrH:1].[Br-].[CH3:3][N+:4]([CH3:11])([CH3:10])[CH2:5][CH2:6][CH2:7][NH:8][CH3:9].[OH-].[Na+]>CO>[Br-:1].[CH3:3][N+:4]([CH3:11])([CH3:10])[CH2:5][CH2:6][CH2:7][NH:8][CH3:9]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 20320282N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide

Produkt 1

HCID 21444211N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

To a stirred suspension of 876.0 g. (3.0 moles) of N,N,N,-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide in 2.75 liters of absolute methanol at room temperature is added a freshly prepared solution of sodium hydroxide (120.0 g., 3.0 moles) in 1.0 liter of absolute methanol over a period of 1.0 hour. The reaction mixture is evaporated under reduced pressure and the solid residue is shaken with 750 ml. of acetonitrile. The insoluble sodium bromide is removed by filtration and the filtrate is evaporated. The solid residue is dried in vacuo to give a quantitative yield of white, crystalline hygroscopic product which may be used without further purification or can be recrystallized from isopropanol-ether. NMR (D2O) δ: 2.28 (3H, S, --NHCH3); 3.11 (9H, S, --+N(CH3)3).

Aufarbeitung

  1. additionTo a stirred suspension of 876.0 g
  2. customThe reaction mixture is evaporated under reduced pressure
  3. customThe insoluble sodium bromide is removed by filtration
  4. customthe filtrate is evaporated
  5. customThe solid residue is dried in vacuo
  6. customto give a quantitative yield of white, crystalline hygroscopic product which
  7. custommay be used without further purification
  8. customcan be recrystallized from isopropanol-ether

Quellen und Nachweise

ORD-Eintrag
ord-b6dcb70210ef499da27dbd61b23b6722
Quelldatensatz
uspto-grants-1978_07
Patentnummer
US04098726

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