HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 60735499, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,5-Dichloropyridine | HCID 27685 | — |
| Reactant | 2-Mercaptopropionate | HCID 15607736 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 60735499 | HCID 60735499 | 76.6% |
Reaction Steps
To a solution of 2,5-dichloropyridine (13, 2.04 g, 13.8 mmol) in 40 mL of dry DMF was added K2CO3 (1.91 g, 13.8 mmol) and reaction mixture was stirred for 30 min at ambient temperature. Neat methylthioglycolate (1.26 mL, 14 mmol) was added via syringe and the reaction mixture was stirred overnight under N2. The reaction mixture was treated with H2O (120 mL) and the product was extracted into EtOAc (2×220 mL). Combined organic layers were washed with lot of water, brine, dried over Na2SO4, filtered and concentrated to give 2.3 g of crude material which was purified by column chromatography (hexanes/EtOAc). Obtained 1.1 g (5.0 mmol) of target 14, as a colorless oil, in 36% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07998980B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-683ed55238ef441a89611373bc16e849 |
| Source note | uspto-grants-2011_08 |