HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86631142, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 67415336 | HCID 67415336 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86631142 | HCID 86631142 | 68% |
Reaction Steps
To a solution of 2-[(2,2-dimethoxy-1-methylethoxy)methyl]pyridine (1.66 g, 7.85 mmol, obtained from Example 20(a)) in THF (30 mL) was added water (10 mL) and concentrated sulfuric acid (1 mL) and the resulting solution was refluxed for 12 h. After cooling to r.t., the volatile components were removed in vacuo and dichloromethane was added followed by saturated sodium bicarbonate solution until the aqueous layer was pH 7. The layers were separated and the aqueous phase was extracted with dichloromethane. The organic layers were combined, dried over sodium sulfate, filtered and concentrated yielding 0.875 g (68% yield) of the title compound. This material was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08026244B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-db2e2fa7f4cb4084808f26d0be1108ff |
| Source note | uspto-grants-2011_09 |