HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 15480787, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 15480786 | HCID 15480786 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 15480787 | HCID 15480787 | 86% |
Reaction Steps
To a solution of Compound 1b (6.4 g, 17 mmol) obtained in Step B in 1,2-dimethoxyethane (96 mL) was added 60% sodium hydride (2.0 g, 50 mmol). After refluxing for 3 hours, the mixture was allowed to cool, poured into ice water, 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=2/1) to give Compound 1c (5.0 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-04129450d5aa4340a7b2c70b87866a33 |
| Source note | uspto-grants-2002_04 |