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Triethylamine → 2,2-difluoro-N-methoxy-N-methylcyclopropane-1-carboxamide

HRID 561445
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 561445
[F:1][C:2]1([F:8])[CH2:4][CH:3]1[C:5](Cl)=[O:6].FF.Cl.[CH3:12][NH:13][O:14][CH3:15].C(N(CC)CC)C>ClCCl.O>[F:1][C:2]1([F:8])[CH2:4][CH:3]1[C:5]([N:13]([O:14][CH3:15])[CH3:12])=[O:6]
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Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 24524FluorineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 150990752,2-Difluorocyclopropane-1-carbonyl chloride

Produkt 1

HCID 534161312,2-difluoro-N-methoxy-N-methylcyclopropane-1-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

7.00 g (49.8 mmol) of 2,2-difluorocyclopropanecarbonyl chloride (described in the Journal of Fluorine Chemistry 1990, 49, 127-139) in 100 ml of dichloromethane were mixed with 6.32 g (64.8 mmol) of N,O-dimethylhydroxylamine hydrochloride and 18.1 ml (130 mmol) of triethylamine and stirred at RT overnight. Water was added to the reaction mixture, the phases were separated, and the aqueous phase was extracted twice with dichloromethane. The combined organic phases were dried over sodium sulfate and concentrated. 5.73 g (70% of theory) of the title compound were obtained and were reacted without further purification.

Aufarbeitung

  1. customthe phases were separated
  2. extractionthe aqueous phase was extracted twice with dichloromethane
  3. dry with materialThe combined organic phases were dried over sodium sulfate
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-481566167d8947818e363c2f0c197f81
Quelldatensatz
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08063234B2

Notizen zur Reaktion

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