HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 3-Chloro-6'-methyl-5-vinyl-2,3'-bipyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-Methylpyridine-5-boronic acid | HCID 2763081 | — |
| Reactant | 2,3-Dichloro-5-ethenylpyridine | HCID 57416849 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 3-Chloro-6'-methyl-5-vinyl-2,3'-bipyridine | HCID 57825702 | 90.2% |
Reaction Steps
8.1 g of Na2CO3 (76 mmol), 3.5 g of 6-methylpyridin-3-ylboronic acid (11) (25 mmol), and 0.97 g of Pd(PPh3)4 were added to 4.9 g of compound (8) (28 mmol) prepared in Example 5 dissolved in 100 mL of 1,2-dimethoxyethane and 100 mL of distilled water, and refluxed under heating and stirring for 18 hours. The mixture was cooled to room temperature, and concentrated about 50% under reduced pressure. The aqueous layer was extracted with ethyl acetate, and the organic layer was dried over magnesium sulfate, concentrated under reduced pressure. The residue was separated by column chromatography (eluting solvent: ethyl acetate/hexane=1/4) to obtain 5.2 g of 3-chloro-6′-methyl-5-vinyl-2,3′-bipyridine (yield 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08940769B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-e2d6c5f85b5d4de7a534c6766831e6a0 |
| Source note | uspto-grants-2015_01 |