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Water → 2-(5-Cyano-3,4-diphenyl-6-oxo-1,6-dihydropyridazin-1-yl) ethyl sulfonic acid hydrate

HRID 463972
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 463972
[C:1]([C:3]1[C:4](=[O:21])[NH:5][N:6]=[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)#[N:2].C([O-])([O-])=O.[K+].[K+].O.[Na+].Br[CH2:31][CH2:32][S:33]([O-:36])(=[O:35])=[O:34]>CN(C=O)C>[OH2:21].[C:1]([C:3]1[C:4](=[O:21])[N:5]([CH2:31][CH2:32][S:33]([OH:36])(=[O:35])=[O:34])[N:6]=[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)#[N:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 957574-Pyridazinecarbonitrile, 2,3-dihydro-3-oxo-5,6-diphenyl-HCID 236667972-Bromoethanesulfonic acid, sodium salt

Produkt 1

HCID 135335102-(5-Cyano-3,4-diphenyl-6-oxo-1,6-dihydropyridazin-1-yl) ethyl sulfonic acid hydrateAusbeute 50,1 %

Reagenzien, Katalysatoren, Lösungsmittel

1
HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

7.5 grams (0.027 mole) of the product of Example 1 was caused to react with 3.79 grams of K2CO3 in the least amount of water along with 200 mls of DMF. To this mixture was added 5 drops of 18 crown-6-ether. Into this solution was added 5.79 grams (0.027 mole) of 2-bromoethane sulfonic acid sodium salt and the mixture heated to 110° C. for 3 hours. The solution was filtered and the filtrate was distilled at reduced pressure. The residual solid was dissolved in excess water and poured into conc. hydrochloric acid. The solid that precipitated was filtered and washed with water and then air dried. The recovered solid was recrystallized from acetonitrile to give 2.7 grams of a yellow solid which melted at 138°-140° C.

Aufarbeitung

  1. filtrationThe solution was filtered
  2. distillationthe filtrate was distilled at reduced pressure
  3. dissolutionThe residual solid was dissolved in excess water
  4. additionpoured into conc. hydrochloric acid
  5. customThe solid that precipitated
  6. filtrationwas filtered
  7. washwashed with water
  8. customair dried
  9. customThe recovered solid was recrystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-66ac0158d8074536b9b18328140f45bc
Quelldatensatz
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04545810

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