HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22175084, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 3-(benzyloxy)-4,6-dibromopicolinate | HCID 22175074 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22175084 | HCID 22175084 | 95.3% |
Reaction Steps
A vigorously stirred mixture of 15 (25.5 g), potassium carbonate (75 g) and methanol (300 mL) was heated at reflux for 30 hours. The mixture was cooled, poured into water (800 mL), and the pH adjusted to 2 by the addition of conc. HCl. The resulting mixture was extracted with CH2Cl2 (3×150 mL). The organic extracts were combined, dried (MgSO4) and the solvent was evaporated to give a nearly colorless oil (20.5 g) which slowly solidified upon standing. This was recrystallized from methanol (125 mL)/water (40 mL) to give the desired acid 16 (11.6 g), m.p. 134-135° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06927225B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-159353f94c514149aa8d8dbc1b0a7742 |
| Source note | uspto-grants-2005_08 |