Ammonium trifluoroacetate → HCID 178432621, Verbindung

HRID 2367399Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2367399
[CH3:1][CH:2]([NH:11][C:12]([CH:14]1[O:19][CH2:18][CH2:17][N:16]([CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:15]1)=O)[C:3](=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.FC(F)(F)C([O-])=O.[NH4+:34]>>[CH3:1][C:2]1[N:11]=[C:12]([CH:14]2[O:19][CH2:18][CH2:17][N:16]([CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:15]2)[NH:34][C:3]=1[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

Komponenten

3

Edukt 2

HCID 2724268Ammonium trifluoroacetateHCID 58504388N-(1-Methyl-2-oxo-2-phenylethyl)-4-(phenylmethyl)-2-morpholinecarboxamide

Produkt 1

HCID 178432621HCID 178432621, VerbindungAusbeute 97,5 %

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A mixture of N-(1-methyl-2-oxo-2-phenylethyl)-4-(phenylmethyl)-2-morpholinecarboxamide (1.3 g, 3.69 mmol) and ammonium trifluoroacetate (2.417 g, 18.44 mmol) was stirred for 0.75 hours at 150° C. The LCMS indicated that the starting material was consumed. The desired product was contained in the residue. Water (150 mL) was added to the residue, and the resulting mixture was extracted with EtOAc (3×100 mL). The organics were dried (Na2SO4), filtered, and evaporated to afford the title compound (1.2 g) as a brown oil. LC-MS (ES) m/z=334 [M+H]+.

Aufarbeitung

  1. customwas consumed
  2. additionWater (150 mL) was added to the residue
  3. extractionthe resulting mixture was extracted with EtOAc (3×100 mL)
  4. dry with materialThe organics were dried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-6b4055e68b5042bcbca5314743d8fc31
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08697685B2

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