Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Toluene | HCID 1140 | — |
| Edukt | Choline, hydroxide | HCID 31255 | — |
| Edukt | HCID 178418421 | HCID 178418421 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178418456 | HCID 178418456 | 55% |
Reaktionsschritte
To a stirred suspension of 7-chloro-2,3-dihydro-10-hydroxypyridazino[4,5-b]quinoline-1,4-dione (1.00 g, 3.8 mM) in water (40 mL) was added choline hydroxide (0.86 mL, 3.8 mM, 50 weight per cent, aqueous solution). Toluene (250 mL) was added to the resulting solution and the mixture was concentrated using a rotary evaporator. The residue was diluted with toluene (250 mL) and the resulting mixture concentrated again to provide a yellow residue. This residue was stirred for 60 hr with methanol (25 mL) and the resulting suspension was filtered to separate the solids which were washed with methanol (3 mL) and then dried under a stream of nitrogen for 1 hr. Further drying of the solids in vacuo at 100° C. for 20 hr provided (0.76 g, 55%) of the title compound as a yellow powder, mp 267°-269° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05733910 |
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| Quelldatensatz | uspto-grants-1998_03 |
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| ORD ID | ord-4061f90aaff7419f9113b9addf8ac370 |
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| Quellennotiz | uspto-grants-1998_03 |
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