Hydrochloric Acid → 3-(N-Methylpentylamino)propionic acid hydrochloride

HRID 1350596

Reaktionsgleichung

Reaktionsgleichung von HRID 1350596
C[O:2][C:3](=[O:13])[CH2:4][CH2:5][N:6]([CH3:12])[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[ClH:14]>O>[ClH:14].[CH3:12][N:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])[CH2:5][CH2:4][C:3]([OH:13])=[O:2]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 16726422Methyl 3-(methyl(pentyl)amino)propanoate

Produkt 1

HCID 167264233-(N-Methylpentylamino)propionic acid hydrochlorideAusbeute 82,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
24 °C

Versuchsvorschrift

68.8 g (367.4 mmol) N-methyl-N-pentyl-β-alanine methyl ester was hydrolyzed by refluxing with 138 ml water. Then the water is partly distilled off and 83 ml (472.7 mmol) hydrochloric acid (19%) was added. Water was distilled off again and 230 ml methyl ethyl ketone was added to remove residual water by azeotropic distillation. The reaction mixture was then cooled to 24° C. The crystallized product was separated and washed with methyl ethyl ketone and subsequently dried in vacuo. 63.7 g (82.7%) N-methyl-N-pentyl-β-alanine hydrochloride were obtained.

Aufarbeitung

  1. distillationThen the water is partly distilled off
  2. distillationWater was distilled off again
  3. addition230 ml methyl ethyl ketone was added
  4. customto remove residual water
  5. distillationby azeotropic distillation
  6. customThe crystallized product was separated
  7. washwashed with methyl ethyl ketone
  8. customsubsequently dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-744adb86bb3e4a93923a6ff91260a4e5
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07214818B2

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