Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Calcium Chloride | HCID 5284359 | — |
| Reactant | HCID 135599962 | HCID 135599962 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 135600000 | HCID 135600000 | 65.1% |
Reaction Steps
A mixture of 3-amino-2-(2-chloro-5-methoxyphenyl)-7-nitro-2,5-dihydro-4H-pyrazolo[4,3-c]quinolin-4-one (0.50 g), 90% calcium chloride (0.40 g), reduced iron (1.0 g) and 90% ethanol (30 ml) was heated under reflux for 3 hours, and 90% calcium chloride (0.10 g) and reduced iron (0.27 g) was added thereto. The reaction mixture was heated under reflux for additional 8 hours. The reaction mixture was cooled and the insoluble materials were filtered off through Celite, and the filtrate was extracted with ethyl acetate. The extract was washed with a 5% sodium hydrogen carbonate and brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residual solid was washed with diisopropyl ether, and dried to obtain the target compound (0.30 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07842701B2 |
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| Source dataset | uspto-grants-2010_11 |
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| ORD ID | ord-27a491837b55494694f21ef22bfc8a60 |
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| Source note | uspto-grants-2010_11 |
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