HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57791289, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 57791309 | HCID 57791309 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 57791289 | HCID 57791289 | 65.1% |
Reaction Steps
3-Ethoxy-2-fluoro-6-methylpyridine (400 mg) was initially introduced in carbon tetrachloride (30 ml) and, after addition of N-bromosuccinimide (505 mg) and 2,2′-azobis(2-methylpropionitrile) (85 mg), the reaction mixture was heated at reflux for 7 h. After standing overnight at RT, it was treated with water and extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue was purified on silica gel (n-heptane-ethyl acetate gradient). After the combination of the product-containing fractions, it was brought to dryness. 393 mg of the desired compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07863269B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-03517d09f06242d69afc61f8270e78d2 |
| Source note | uspto-grants-2011_01 |