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Hydrochloric Acid → HCID 22025427, Verbindung

HRID 2061637
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2061637
[F:1][C:2]([F:25])([F:24])[CH2:3][NH:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][C:8]=1/[CH:17]=[CH:18]/[C:19]([O:21]CC)=[O:20])=[O:6].[OH-].[Na+].Cl>CO>[O:6]=[C:5]1[C:7]2[C:8](=[CH:9][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:11][CH:12]=2)[CH:17]([CH2:18][C:19]([OH:21])=[O:20])[N:4]1[CH2:3][C:2]([F:25])([F:24])[F:1]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57678952Ethyl (E)-3-[2-(2,2,2-trifluoroethylcarbamoyl)-5-trifluoromethylphenyl]acrylate

Produkt 1

HCID 22025427HCID 22025427, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

2.2 g of ethyl (E)-3-[2-(2,2,2-trifluoroethylcarbamoyl)-5-trifluoromethylphenyl]acrylate (5.9 mmol) were dissolved in 10 ml of methanol and 1.5 ml of a 5 M aqueous NaOH solution (7.5 mmol) were added. The mixture was stirred at RT for 18 h and then set to pH=7 using aqueous HCl solution. The solvents were removed under reduced pressure and the residue was suspended in 10 ml of water. This suspension was set to pH=2 using a 2N aqueous HCl solution and extracted 3 times with 10 ml each time of EA. Drying was effected over Na2SO4 and the solvent was removed under reduced pressure. The residue was crystallized with diethyl ether/DIP, mp: 202-204° C.

Aufarbeitung

  1. customThe solvents were removed under reduced pressure
  2. extractionextracted 3 times with 10 ml each time of EA
  3. customDrying
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was crystallized with diethyl ether/DIP, mp: 202-204° C.

Quellen und Nachweise

ORD-Eintrag
ord-478de4c276bc49469cdfe0325c2241a8
Quelldatensatz
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08283374B2

Notizen zur Reaktion

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