Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Nitric Acid | HCID 944 | — |
| Edukt | Phosphoric Acid | HCID 1004 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Acetylacetone | HCID 31261 | — |
| Edukt | 4-(Morpholinosulfonyl)aniline | HCID 210794 | — |
| Edukt | Potassium Acetate | HCID 517044 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178468359 | HCID 178468359 | 86% |
Reaktionsschritte
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%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08354411B2 |
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| Quelldatensatz | uspto-grants-2013_01 |
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| ORD ID | ord-648dd20b48ab4e63b86bd14c7dc74088 |
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| Quellennotiz | uspto-grants-2013_01 |
|---|