Nitric Acid → HCID 178468359, Verbindung

HRID 1624567

Reaktionsgleichung

[N:1]1([S:7]([C:10]2[CH:16]=[CH:15][C:13]([NH2:14])=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.P(=O)(O)(O)O.[N+]([O-])(O)=O.[N:26]([O-])=O.[Na+].[CH3:30][C:31](=[O:36])[CH2:32][C:33](=[O:35])[CH3:34].C([O-])(=O)C.[K+].C([O-])([O-])=O.[Na+].[Na+]>C(O)C>[N:1]1([S:7]([C:10]2[CH:16]=[CH:15][C:13]([NH:14][N:26]=[C:32]([C:31](=[O:36])[CH3:30])[C:33](=[O:35])[CH3:34])=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH2:2][CH2:3][O:4][CH2:5][CH2:6]1

Komponenten

Reaktionsbedingungen

Temperatur: -6 °C

Versuchsvorschrift

4-(Morpholin-4-ylsulfonyl)aniline (300 mg, 1.24 mmol) was added to a solution of 3 mL of phosphoric acid (85%) and 2 mL of nitric acid (65%) at −6° C. When the mixture reached to room temperature it was cooled to −6° C. and solid sodium nitrite (85 mg, 1.24 mmol) was added during 10 min. Small pieces of ice (50 g) were added into the solution. The mixture was added at 0° C. to a suspension of corresponding 2,4-pentanedione (124 mg, 1.24 mmol) and potassium acetate (20 g) in ethanol (250 mL). The solution was stirred for 15 min, added to 250 mL of a saturated solution of Na2CO3, extracted with dichloromethane, washed with water and brine, dried over Na2SO4, and concentrated under reduced pressure to give 3-{[4-(morpholin-4-ylsulfonyl)phenyl]hydrazono}pentane-2,4-dione (375 mg, 86%).

Aufarbeitung

customreached to room temperature
extractionextracted with dichloromethane
washwashed with water and brine
dry with materialdried over Na2SO4
concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-ca13ca2da7b84d2bbd0f297493a92c34
Quelldatensatz: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08778944B2

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