Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1-[4-(2-methyl-[1,3]dioxolan-2-yl)-thiophen-2-ylmethyl]-4-nitro-1H-pyrazole | HCID 66928880 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67365611 | HCID 67365611 | — |
Reaction Steps
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of 1-[4-(2-methyl-[1,3]dioxolan-2-yl)-thiophen-2-ylmethyl]-4-nitro-1H-pyrazole (115 mg, 0.39 mmol), iron powder (65 mg, 1.16 mmol) and NH4Cl (106 mg, 1.97 mmol) in a mixture of EtOH (3.0 mL) and water (1.5 mL) was stirred at 75° C. for 60 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. The filtrated was dried over Na2SO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a yellow oil: TLC: rf (EA)=0.63. LC-MS-conditions 02: tR=0.76 min; [M+H]+=267.09.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08536209B2 |
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| Source dataset | uspto-grants-2013_09 |
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| ORD ID | ord-d9302624e474456f9d9f8a369a4d5bec |
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| Source note | uspto-grants-2013_09 |
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