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Hydrochloric Acid → 8-ethyl-6-naphthalen-2-yl-2-phenylamino-8H-pyrido[2,3-d]-pyrimidin-7-one

HRID 3235
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 3235
[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([NH:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:11]=[CH:12][C:7]=2[CH:6]=[C:5]([C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:21]=2)[C:4]1=N)[CH3:2].C(OC(=O)C)(=[O:33])C.Cl>O>[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([NH:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:11]=[CH:12][C:7]=2[CH:6]=[C:5]([C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:21]=2)[C:4]1=[O:33])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 11710876(8-Ethyl-7-imino-6-naphthalen-2-yl-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl)-phenylamine

Produkt 1

HCID 115384008-ethyl-6-naphthalen-2-yl-2-phenylamino-8H-pyrido[2,3-d]-pyrimidin-7-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

(8-Ethyl-7-imino-6-naphthalen-2-yl-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl)-phenylamine (150 mg) was added to 1 mL of acetic anhydride and heated at reflux for 2 minutes. The reaction was cooled and concentrated, resulting in an oil which was heated at reflux with 10 mL of 6N HCl for 10 minutes. The reaction was cooled, and 40 mL of water was added causing precipitation. The precipitate was removed by filtration and washed with water. The resulting solid was dried in a vacuum oven to provide 8-ethyl-6-naphthalen-2-yl-2-phenylamino-8H-pyrido[2,3-d]-pyrimidin-7-one; mp 254°-256° C.

Aufarbeitung

  1. temperatureheated
  2. temperatureat reflux for 2 minutes
  3. temperatureThe reaction was cooled
  4. concentrationconcentrated
  5. customresulting in an oil which
  6. temperaturewas heated
  7. temperatureThe reaction was cooled
  8. customprecipitation
  9. customThe precipitate was removed by filtration
  10. washwashed with water
  11. customThe resulting solid was dried in a vacuum oven

Quellen und Nachweise

ORD-Eintrag
ord-bbffcf2db8554d41a139114578bcbcd5
Quelldatensatz
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05733914

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