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Chloroacetic Acid → HCID 43700001, Verbindung

HRID 2062078
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2062078
[Cl:1][CH2:2][C:3](O)=[O:4].[CH3:6][O:7][C:8](=[O:13])[C:9]([NH2:12])([CH3:11])[CH3:10].C(N(CC)C(C)C)(C)C>C1COCC1>[CH3:6][O:7][C:8](=[O:13])[C:9]([NH:12][C:3](=[O:4])[CH2:2][Cl:1])([CH3:11])[CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 300Chloroacetic AcidHCID 81531DiisopropylethylamineHCID 4186341Methyl 2-amino-2-methylpropanoate

Produkt 1

HCID 43700001HCID 43700001, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 0.95 g chloro acetic acid in 20 ml of dry THF 1.78 g N,N′-carbonyl-diimidazole were added. After 0.5 h at room temperature and under argon atmosphere 1.69 g 2-amino-2-methyl-propionic acid methyl ester and 1.29 g N,N-diisopropyl-ethyl-amine were added and it was stirred for 3 h. Then the solvent was evaporated, the residue taken up in ethyl acetate and washed with 2 M hydrochloric acid, water and sat. aqueous sodium hydrogen carbonate solution. The combined organic fractions were dried over sodium sulphate, filtrated and concentrated. The resulting residue was crystallized from diethylether to yield 2-(2-chloro-acetylamino)-2-methyl-propionic acid methyl ester.

Aufarbeitung

  1. customThen the solvent was evaporated
  2. washwashed with 2 M hydrochloric acid, water and sat. aqueous sodium hydrogen carbonate solution
  3. dry with materialThe combined organic fractions were dried over sodium sulphate
  4. filtrationfiltrated
  5. concentrationconcentrated
  6. customThe resulting residue was crystallized from diethylether

Quellen und Nachweise

ORD-Eintrag
ord-aaffaad8fc7f4287a35f12dfdfab8013
Quelldatensatz
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08283479B2

Notizen zur Reaktion

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