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Sodium Hydroxide → 3-Propyl-2lambda~6~-pyrido[2,3-c][1,2,6]thiadiazine-2,2,4(1H,3H)-trione

HRID 66042
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 66042
[CH2:1]([NH:4][S:5]([NH:8][C:9]1[C:14]([C:15]([O:17]C)=O)=[CH:13][CH:12]=[CH:11][N:10]=1)(=[O:7])=[O:6])[CH2:2][CH3:3].[OH-].[Na+]>O>[CH2:1]([N:4]1[S:5](=[O:7])(=[O:6])[NH:8][C:9]2[N:10]=[CH:11][CH:12]=[CH:13][C:14]=2[C:15]1=[O:17])[CH2:2][CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 22756776HCID 22756776, Verbindung

Produkt 1

HCID 227567853-Propyl-2lambda~6~-pyrido[2,3-c][1,2,6]thiadiazine-2,2,4(1H,3H)-trione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Methyl 2-(((n-propylamino)sulfonyl)amino)- 3-pyridinecarboxylate (15.7 grams; 0.057 mole), 95 ml of water and 10.5 ml of 50 percent aqueous sodium hydroxide were mixed and the resulting reaction mixture stirred for about one and one-fourth hours at ambient temperatures. The reaction mixture was extracted with two - 50 ml portions of methylene chloride and one - 50 ml portion of ether to remove impurities. The aqueous layer was separated from the organic layer and acidified to a pH of about 4.5 with concentrated hydrochloric acid. The solution was filtered and the filtrate to a pH of about 1. The resulting product precipitate was recovered by filtration, dissolved in acetone and the solution filtered and dried with magnesium sulfate. The mixture was again filtered and the filtrate reduced in vacuo to obtain the title compound as a yellow powder having a melting point of 208° C-210° C.

Aufarbeitung

  1. customthe resulting reaction mixture
  2. extractionThe reaction mixture was extracted with two - 50 ml portions of methylene chloride and one - 50 ml portion of ether
  3. customto remove impurities
  4. customThe aqueous layer was separated from the organic layer
  5. filtrationThe solution was filtered
  6. filtrationThe resulting product precipitate was recovered by filtration
  7. dissolutiondissolved in acetone
  8. filtrationthe solution filtered
  9. dry with materialdried with magnesium sulfate
  10. filtrationThe mixture was again filtered

Quellen und Nachweise

ORD-Eintrag
ord-96fa9cdc7fd94ff59ec3984879894493
Quelldatensatz
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04129733

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