HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86626289, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Isobutylamine | HCID 6558 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,4-Dichloro-5,6-dimethyl-3-nitropyridine | HCID 12109123 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86626289 | HCID 86626289 | — |
Reaction Steps
A modification of the method described in Part A of Example 4 was used to treat 2,4-dichloro-5,6-dimethyl-3-nitropyridine (Dellaria et al, U.S. Pat. No. 6,545,016, Example 7, Part A, 50.0 g, 0.194 mol) with triethylamine (47 mL, 0.34 mol) and isobutylamine (27 mL, 0.27 mol) in anhydrous DMF (500 mL). The work-up procedure was as follows. The reaction mixture was poured into hot water (1 L). The resulting mixture was extracted with chloroform (2×800 mL), and the combined extracts were dried over magnesium sulfate, filtered through a layer of CELITE filter agent, and concentrated under reduced pressure to provide 60.78 g of 2-chloro-5,6-dimethyl-4-(2-methylpropyl)-3-nitropyridine as a bright orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08143270B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-8c79855a20614917a8a0b5621bc60d14 |
| Source note | uspto-grants-2012_03 |