HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22616364, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 22616353 | HCID 22616353 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 22616364 | HCID 22616364 | 86.6% |
Reaction Steps
To a solution of Compound 12b (11 g, 27 mmol) obtained in Step B in 1,2-dimethoxyethane (161 mL) was added 60% sodium hydride (3.3 g, 83 mmol). After refluxing for 3 hours, the mixture was allowed to cool and poured into ice water, and the mixture was acidified with 6 mol/L hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with brine and dried over sodium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography (eluted with hexane/ethyl acetate=3/1) to give Compound 12c (8.4 g, 86%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376535B2 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-e8273eab754746f59696a16c8ab7b808 |
| Source note | uspto-grants-2002_04 |