Methylamine → N-Methyl-2-(1-methyl-1H-pyrazol-4-yl)ethan-1-amine

HRID 385889

Reaktionsgleichung

Reaktionsgleichung von HRID 385889
Cl[CH2:2][CH2:3][C:4]1[CH:5]=[N:6][N:7]([CH3:9])[CH:8]=1.[CH3:10][NH2:11]>>[CH3:10][NH:11][CH2:2][CH2:3][C:4]1[CH:5]=[N:6][N:7]([CH3:9])[CH:8]=1

Komponenten

3

Edukt 2

HCID 6329MethylamineHCID 595256864-(2-chloroethyl)-1-methyl-1H-pyrazole

Produkt 1

HCID 51000371N-Methyl-2-(1-methyl-1H-pyrazol-4-yl)ethan-1-amine

Versuchsvorschrift

To neat 4-(2-chloroethyl)-1-methyl-1H-pyrazole (50 g, 0.24 mol) was added a 25% aqueous solution of methylamine (1.15 L, 7.21 mol). The mixture was placed into an autoclave at 60° C. for 15 h. The resulting mixture was concentrated in vacuo, treated with aqueous solution of NaOH and extracted with DCM. The combined organic layers were concentrated in vacuo and purified by vacuum distillation to afford the title compound. b.p. 89-90° C./2 mm Hg.

Aufarbeitung

  1. concentrationThe resulting mixture was concentrated in vacuo
  2. additiontreated with aqueous solution of NaOH
  3. extractionextracted with DCM
  4. concentrationThe combined organic layers were concentrated in vacuo
  5. distillationpurified by vacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-6e4fd895a7144b869cd4b77e9541f4cc
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08367706B2

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