2,2,2-Trifluoroethylamine hydrochloride → Ethanimidic acid, N-(2,2,2-trifluoroethyl)-, ethyl ester

HRID 1367731Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1367731
Cl.[C:2](=[NH:7])([O:4][CH2:5][CH3:6])[CH3:3].Cl.[F:9][C:10]([F:14])([F:13])[CH2:11]N.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl.O>[CH2:5]([O:4][C:2](=[N:7][CH2:11][C:10]([F:14])([F:13])[F:9])[CH3:3])[CH3:6]

Komponenten

6

Edukt 3

HCID 97722,2,2-Trifluoroethylamine hydrochlorideHCID 11430Potassium CarbonateHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)

Produkt 1

HCID 86618848Ethanimidic acid, N-(2,2,2-trifluoroethyl)-, ethyl esterAusbeute 87,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Ethyl acetimidate hydrochloride (1.23 g, 9.95 mmol) and 2,2,2-trifluoroethylamine hydrochloride (1.35 g, 9.95 mmol) were dissolved in CH2Cl2 (32 mL)/H2O (3.2 mL). K2CO3 (0.69 g, 4.98 mmol) was added and stirred for 30 minutes. The two layers were separated. The aqueous layer was extracted with CH2Cl2 (2×10 mL). The combined organic layer was dried with Na2SO4 and concentrated to give 1.48 g of N-(2,2,2-Trifluoro-ethyl)-acetimidic acid ethyl ester as a light yellow liquid in 87% yield.

Aufarbeitung

  1. customThe two layers were separated
  2. extractionThe aqueous layer was extracted with CH2Cl2 (2×10 mL)
  3. dry with materialThe combined organic layer was dried with Na2SO4
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-6d89aca6f678432e82a6d51e32ea06fb
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07893264B2

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