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Sodium Hydroxide → 2,2,7-Trimethyl-1,3-dioxolo-[4,5-g]-quinoxaline-6-carboxylic acid, 1,1-dimethylethyl ester

HRID 725246
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 725246
[NH2:1][C:2]1[C:12]([NH2:13])=[CH:11][C:5]2[O:6][C:7]([CH3:10])([CH3:9])[O:8][C:4]=2[CH:3]=1.C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl.[OH-].[Na+].[C:30]([O:34][C:35](=[O:41])[C:36](=O)[C:37](=O)[CH3:38])([CH3:33])([CH3:32])[CH3:31]>O.O1CCCC1>[CH3:9][C:7]1([CH3:10])[O:6][C:5]2=[CH:11][C:12]3[N:13]=[C:37]([CH3:38])[C:36]([C:35]([O:34][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:41])=[N:1][C:2]=3[CH:3]=[C:4]2[O:8]1
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Komponenten

7

Edukt 4

HCID 14798Sodium HydroxideHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 10986731Tert-butyl 2,3-dioxobutanoateHCID 13343758HCID 13343758, Verbindung

Produkt 1

HCID 540074732,2,7-Trimethyl-1,3-dioxolo-[4,5-g]-quinoxaline-6-carboxylic acid, 1,1-dimethylethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

[5,6-diamino-2,2-dimethyl-1,3-benzodioxole; dihydrochloride salt] (U.S. Pat. No. 4,904,775, Example 3D) (6.8 g, 0.02 mmol) was dissolved in a mixture of 25 ml water and 10 ml tetrahydrofuran and the pH of the solution was adjusted to 5.5 by the addition of 2N NaOH. After addition of the compound from Example 1 (3.8 g; 0.02 mol) the mixture was refluxed for 2 hours, concentrated in vacuo to remove the organic solvent tetrahydrofuran and then extracted with ethyl acetate. The combined organic phases were washed with brine, dried (Na2SO4) and then evaporated in vacuo to leave an oil which crystallized by the addition of petroleum ether. M.P. 104°-105° C.; yield 5.2 g (82%). C17H20N2O4 % C calc. 64.54%, found 64.40% % H calc. 6.37%, found 6.41% % N calc. 8.85%, found 8.86%

Aufarbeitung

  1. temperaturewas refluxed for 2 hours
  2. concentrationconcentrated in vacuo
  3. customto remove the organic solvent tetrahydrofuran
  4. extractionextracted with ethyl acetate
  5. washThe combined organic phases were washed with brine
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo
  8. customto leave an oil which
  9. customcrystallized by the addition of petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-699b74c1d37f48d3956f8cfc88094db9
Quelldatensatz
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05705645

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