Hydrochloric Acid → HCID 12850756, Verbindung

HRID 1395041Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1395041
C([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]=[CH:12][C:13]3[C:19](=[O:20])[C:18]([C:21]([O:23]CC)=[O:22])=[CH:17][NH:16][C:14]=3[N:15]=2)[CH2:6][CH2:5]1)(=O)C.Cl>O.C(O)C>[N:7]1([C:10]2[N:11]=[CH:12][C:13]3[C:19](=[O:20])[C:18]([C:21]([OH:23])=[O:22])=[CH:17][NH:16][C:14]=3[N:15]=2)[CH2:6][CH2:5][NH:4][CH2:9][CH2:8]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 12917681Ethyl 2-(4-acetyl-1-piperazinyl)-5,8-dihydro-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate

Produkt 1

HCID 12850756HCID 12850756, VerbindungAusbeute 78,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A suspension of ethyl 5,8-dihydro-2-(4-acetyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate (1000 g) and concentrated hydrochloric acid (800 ml) in a mixture of water (1200 ml) and ethanol (1000 ml) was refluxed for 8 hours and allowed to stand overnight. The crystals precipitated were collected, washed with ethanol, and dissolved by heating in an aqueous solution (10 liters) of sodium hydroxide (250 g). The solution was filtered, adjusted to pH 7-8 with acetic acid, and allowed to stand overnight with ice-cooling. The crystalline precipitate was collected, washed with water, and dried at 110° C. to give 5,8-dihydro-2-(1-piperazinyl)-5-oxopyrido [2,3-d]pyrimidine-6-carboxylic acid (625 g). m.p. 299°-305° C. (decomp.).

Aufarbeitung

  1. temperaturewas refluxed for 8 hours
  2. customThe crystals precipitated
  3. customwere collected
  4. washwashed with ethanol
  5. dissolutiondissolved
  6. temperatureby heating in an aqueous solution (10 liters) of sodium hydroxide (250 g)
  7. filtrationThe solution was filtered
  8. waitto stand overnight with ice-
  9. temperaturecooling
  10. customThe crystalline precipitate was collected
  11. washwashed with water
  12. customdried at 110° C.

Quellen und Nachweise

ORD-Eintrag
ord-42f90dcbb8e648d994227d86eda3b2f5
Quelldatensatz
uspto-grants-1980_05
Patentnummer
US04201781

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