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Benzaldehyde → HCID 67213120, Verbindung

HRID 2223827
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2223827
Cl[C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH3:11])[CH3:10])[N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:3]=1.CN(C)C=O.[F:24][C:25]1[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=1[NH2:27].Cl.O1CCOCC1.C(O)C(N)(CO)CO.C(=O)C1C=CC=CC=1.C(=O)(O)[O-].[Na+]>CN1CCCC1=O.C(Cl)(Cl)Cl>[F:24][C:25]1[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=1[NH:27][C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH3:11])[CH3:10])[N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 240BenzaldehydeHCID 6503Tris(hydroxymethyl)aminomethaneHCID 516892Sodium BicarbonateHCID 7907666-Chloro-N2-isopropyl-N4-phenyl-1,3,5-triazine-2,4-diamineHCID 204431481,4-Dioxane hydrochlorideHCID 23033167HCID 23033167, Verbindung

Produkt 1

HCID 67213120
HCID 67213120, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A 14 mg portion of 6-chloro-N-isopropyl-N′-phenyl-1,3,5-triazine-2,4-diamine was dissolved in 800 μl of N-methyl-2-pyrrolidone, and 200 μl of 0.5 mM 2-fluoroaniline N,N-dimethylformamide solution and 50 μl of 4 M hydrochloric acid/dioxane were added thereto and stirred at 80° C. for 7 hours. After cooling down the reaction solution to 60° C., 50 mg (4.27 mmol/g) of PS-trisamine and 50 mg (1.53 mmol/g) of PS-benzaldehyde both manufactured by Algonote were added to the reaction solution and further stirred at 60° C. for 16 hours. The reaction solution was cooled down to room temperature and then mixed with saturated sodium bicarbonate aqueous solution and chloroform and stirred. After filtration of the solution, the organic layer was dried using anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure to obtain 13 mg of N-(2-fluorophenyl)-N′-isopropyl-N″-phenyl-1,3,5-triazine-2,4,6-triamine as a brown resinous substance.

Aufarbeitung

  1. temperatureAfter cooling down the reaction solution to 60° C.
  2. additionwere added to the reaction solution
  3. stirringfurther stirred at 60° C. for 16 hours
  4. temperatureThe reaction solution was cooled down to room temperature
  5. stirringstirred
  6. filtrationAfter filtration of the solution
  7. customthe organic layer was dried
  8. customthe solvent was evaporated under a reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-adfed781310f452c884a0e15a1bcb7d7
Quelldatensatz
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07375222B2

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