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Sodium Carbonate → N-[2-(4-nitro-2-methylphenylamino)ethyl]-2,2,2-trifluoroacetamide

HRID 970235
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 970235
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].C(=O)([O-])[O-].[Na+].[Na+].Cl.[F:19][C:20]([F:28])([F:27])[C:21]([NH:23][CH2:24][CH2:25][NH2:26])=[O:22].CN1CCCC1=O>O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([NH:26][CH2:25][CH2:24][NH:23][C:21](=[O:22])[C:20]([F:28])([F:27])[F:19])=[C:3]([CH3:11])[CH:4]=1)([O-:10])=[O:9]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 10340Sodium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 68001Benzene, 1-fluoro-2-methyl-4-nitro-HCID 23021610N-(2-aminoethyl)-2,2,2-trifluoroacetamide hydrochloride

Produkt 1

HCID 23104329N-[2-(4-nitro-2-methylphenylamino)ethyl]-2,2,2-trifluoroacetamideAusbeute 65,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

1.55 g (0.01 mol) of 2-fluoro-5-nitrotoluene, 2.65 g (0.025 mol) of sodium carbonate, 2.11 g (0.011 mol) of 2-(trifluoroacetamido)ethylamine hydrochloride and 10 ml of N-methyl-pyrrolidone were introduced into a three-necked flask under nitrogen. The mixture was heated to 90° C. After reaction for 48 hours, the reaction mixture was cooled and 30 ml of distilled water were then added slowly with vigorous stirring. A yellow precipitate appeared. This precipitate was filtered off, washed several times with water and then with pentane, and dried under vacuum. 1.9 g of expected nitro derivative (1) were obtained in the form of a yellow powder.

Aufarbeitung

  1. customAfter reaction for 48 hours
  2. temperaturethe reaction mixture was cooled
  3. filtrationThis precipitate was filtered off
  4. washwashed several times with water
  5. dry with materialwith pentane, and dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-30b2ebf634ba4af2924cdcd55c2bb20e
Quelldatensatz
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07311737B2

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