Hydrochloric Acid → 4-[(Methoxycarbonyl)(methyl)amino]butanoic acid

HRID 459049Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 459049
Cl.[CH3:2][NH:3][CH2:4][CH2:5][CH2:6][C:7]([OH:9])=[O:8].C(=O)([O-])[O-].[K+].[K+].Cl[C:17]([O:19][CH3:20])=[O:18].Cl>O.O1CCOCC1>[CH3:20][O:19][C:17]([N:3]([CH3:2])[CH2:4][CH2:5][CH2:6][C:7]([OH:9])=[O:8])=[O:18]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 6586Methyl chloroformateHCID 11430Potassium CarbonateHCID 126266544-(Methylamino)butyric acid hydrochloride

Produkt 1

HCID 184429704-[(Methoxycarbonyl)(methyl)amino]butanoic acidAusbeute 170,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4-(Methylamino)butyric acid hydrochloride (5 g, 32.5 mmol), and potassium carbonate (18 g, 130 mmol) were suspended in water (50 ml) and dioxane (25 ml) then cooled to 0° C. Methyl chloroformate (13 ml, 168 mmol) was added over 1 minute, then the mixture was stirred and allowed to warm slowly to room temperature for 16 hours. Conc. HCl (20 ml) was added then the mixture was diluted with water and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, evaporated and dried in vacuo to give 4-[(methoxycarbonyl)(methyl)amino]butyric acid as a thick clear oil (9.7 g).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. customevaporated
  4. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-17349bdd874948b3a3394414256d671c
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07192974B2

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