Water → HCID 178481250, Verbindung

HRID 236243

Reaktionsgleichung

Reaktionsgleichung von HRID 236243
[O-]CC.[Na+].[Na].[H][H].[F:8][C:9]([F:20])([F:19])[C:10]1[CH:11]=[C:12]([CH2:16][C:17]#[N:18])[CH:13]=[CH:14][CH:15]=1.[CH3:21][NH:22][CH:23]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:24](OC)=O.[O-]CC.[Na+].C(O)C.[OH2:41]>C(O)C>[CH3:21][N:22]1[C:17]([NH2:18])=[C:16]([C:12]2[CH:13]=[CH:14][CH:15]=[C:10]([C:9]([F:8])([F:19])[F:20])[CH:11]=2)[C:24](=[O:41])[CH:23]1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

Komponenten

9

Edukt 7

HCID 962WaterHCID 75360m-TrifluoromethylphenylacetonitrileHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 13852358Methyl 2-(methylamino)-2-phenylacetateHCID 23706232Ethanol sodium ethoxideHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 178481250HCID 178481250, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

In this example, sodium ethoxide was prepared by mixing 3.0 g of metallic sodium with 100 ml of absolute ethanol. After the evolution of hydrogen stopped, a mixture containing 16.0 g of (3-trifluoromethylphenyl)-acetonitrile and 17.1 g of methyl methylamino-phenylacetate was added dropwise to the sodium ethoxide-ethanol mixture. The resulting mixture was then refluxed overnight (about 16 hours) and then cooled to room temperature. The mixture was then added to 300 ml of water and extracted with diethyl ether. The ethyl ether extract was filtered to remove precipitate. The filtrate was concentrated by evaporation affording a solid. This solid was then triturated in ethyl ether. The ethyl ether was then removed from the solid. The solid was washed several times with ethyl ether and then dried overnight affording 6.2 g of the title compound.

Aufarbeitung

  1. temperatureThe resulting mixture was then refluxed overnight (about 16 hours)
  2. extractionextracted with diethyl ether
  3. extractionThe ethyl ether extract
  4. filtrationwas filtered
  5. customto remove precipitate
  6. concentrationThe filtrate was concentrated by evaporation
  7. customaffording a solid
  8. customThis solid was then triturated in ethyl ether
  9. customThe ethyl ether was then removed from the solid
  10. washThe solid was washed several times with ethyl ether
  11. customdried overnight

Quellen und Nachweise

ORD-Eintrag
ord-87c51af8ec874c3ea49862dcb3db61f7
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04643762

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