HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 21882728, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 21882699 | HCID 21882699 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 21882728 | HCID 21882728 | 51.1% |
Reaction Steps
0.145 g of ferric chloride and 0.12 g of activated charcoal are added to a suspension of 0.98 g of 2-amino-5-(4-bromphenyl)-3-nitropyridine (starting material H2) in 30 ml of methanol and the mixture is heated under reflux. 0.725 ml of hydrazine hydrate are added slowly and reflux is continued for 24 hours. After cooling the mixture is filtered and the filtrate is evaporated. The residue is partitioned between sodium-EDTA-solution (0.25M; pH 9–10) and dichloromethane. The organic phase is evaporated to give 0.45 g of the title compound as a yellowish solid of m.p. 187–188° C. The mass spectrum shows the molecular peak MH+ at 264.2 Da.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07138399B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-6addb36814c74a7b9b850bf5bca5e634 |
| Source note | uspto-grants-2006_11 |