HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-[(6-Chloropyridin-3-yl)methyl]-2-methylmalonic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Dimethyl 2-[(6-chloropyridin-3-yl)methyl]-2-methylmalonate | HCID 59215199 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-[(6-Chloropyridin-3-yl)methyl]-2-methylmalonic acid | HCID 54283815 | 95% |
Reaction Steps
To a stirred solution of dimethyl 2-[(6-chloropyridin-3-yl)methyl]-2-methylmalonate (10.85 g, 40 mmol) in THF (80 mL) was added a solution of lithium hydroxide monohydrate (5.7 g, 0.136 mol) in water (43 mL). The resulting mixture was stirred overnight at room temperature and then poured into water (300 mL). The pH was adjusted to less than 2 by the addition of concentrated HCl. The resulting mixture was extracted with ether (3×100 mL) and the ether extracts were combined, washed with brine (100 mL) and dried over anhydrous MgSO4. After a filtration, the solvent was evaporated to give 9.26 g of the product as a white solid in 95% yield: m.p. 168° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07795456B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-515a8df1d73a45b6ae219d4c01d500e6 |
| Source note | uspto-grants-2010_09 |