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Sulfuric Acid → HCID 23193696, Verbindung

HRID 48242
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 48242
[CH3:1][N:2]1[CH2:17][CH2:16][C:5]2[C:6]3[NH:7][C:8](=[O:15])[C:9](=[O:14])[NH:10][C:11]=3[CH:12]=[CH:13][C:4]=2[CH2:3]1.[N+:18]([O-])([O-:20])=[O:19].[K+].[OH-].[NH4+].[S:25](=[O:29])(=O)([OH:27])[OH:26]>>[CH3:1][S:25]([OH:27])(=[O:29])=[O:26].[CH3:1][N:2]1[CH2:17][CH2:16][C:5]2[C:6]3[NH:7][C:8](=[O:15])[C:9](=[O:14])[NH:10][C:11]=3[CH:12]=[C:13]([N+:18]([O-:20])=[O:19])[C:4]=2[CH2:3]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 24434Potassium NitrateHCID 104438838-Methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione

Produkt 1

HCID 23193696HCID 23193696, VerbindungAusbeute 35 %

Versuchsvorschrift

A solution of the product from Example 22 (1.07 g,4.7 mmol) was dissolved in 20 ml sulfuric acid. Potassium nitrate (0.51 g, 5.0 mmol) was added in one portion, and the solution stirred for 1 hour. The solution was poured onto ice and made basic with ammonium hydroxide. The yellow solid which formed was filtered and washed with water and ether. The solid was purified by crystallization from water. The solid was suspended in water/DMF and 0.5 g methane sulphonic acid was added. The solution was concentrated, and the solid suspended in acetone, filtered and dried under vacuum (100° C.) to give the title compound (0.60 g, 35% yield), mp=292-294° C.

Aufarbeitung

  1. additionThe solution was poured onto ice
  2. customThe yellow solid which formed
  3. filtrationwas filtered
  4. washwashed with water and ether
  5. customThe solid was purified by crystallization from water
  6. addition0.5 g methane sulphonic acid was added
  7. concentrationThe solution was concentrated
  8. filtrationfiltered
  9. customdried under vacuum (100° C.)

Quellen und Nachweise

ORD-Eintrag
ord-1cef07d946714503aee78dd53a48cb03
Quelldatensatz
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06703391B2

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