Acetic Acid → HCID 19035986, Verbindung

HRID 263903Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 263903
Cl[CH:2]1[C:14]2[NH:13][C:12](=[O:15])[C:11](=[O:16])[NH:10][C:9]=2[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2.[C:17]([OH:20])(=[O:19])[CH3:18]>>[C:17]([O:20][CH:2]1[C:14]2[NH:13][C:12](=[O:15])[C:11](=[O:16])[NH:10][C:9]=2[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2)(=[O:19])[CH3:18]

Komponenten

3

Edukt 2

HCID 176Acetic AcidHCID 19035982HCID 19035982, Verbindung

Produkt 1

HCID 19035986HCID 19035986, VerbindungAusbeute 57,5 %

Versuchsvorschrift

9-Chloro-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione (0.30 g, 1.28 mmol) was refluxed in 50 ml of acetic acid for 10 min. Activated carbon (100 mg) was added and the reaction mixture was filtered and evaporated in vacuo to about 3 ml, and 20 ml of water was added. The precipitate was filtered off and washed with water and dried to give 229 mg of the crude compound, which was recrystallized from acetic acid-water to yield 190 mg (57.5%) of the title compound. M.p.>300° C. 1H-NMR (DMSO-d6, δ): 2.13 (s, 3H), 6.36 (s, 1H), 7.15 (t, 1H), 7.29 (d, 1H) 7.35 (t, 1H), 7.5 (d, 1H), 12.0 (s, 1H), 12.4 (s, 1H).

Aufarbeitung

  1. additionActivated carbon (100 mg) was added
  2. filtrationthe reaction mixture was filtered
  3. customevaporated in vacuo to about 3 ml, and 20 ml of water
  4. additionwas added
  5. filtrationThe precipitate was filtered off
  6. washwashed with water
  7. customdried
  8. customto give 229 mg of the crude compound, which
  9. customwas recrystallized from acetic acid-water

Quellen und Nachweise

ORD-Eintrag
ord-ad6eb70e97de4e0687da9a0c5f56fb44
Quelldatensatz
uspto-grants-1997_07
Patentnummer
US05646146

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