HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69712160, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 131724352 | HCID 131724352 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69712160 | HCID 69712160 | 59% |
Reaction Steps
To a mixture of the product from Step C (0.30 g, 0.78 mmol) in anhydrous THF (20 mL) under nitrogen was added a 1 M solution of lithium aluminum hydride in THF (2.0 mL, 2.6 mmol). The mixture was stirred for 1 h and cooled followed by the addition of methanol and 2 N HCl. The volatiles were evaporated and the residue was purified by reversed phase HPLC (gradient, 0% to 50% acetonitrile in water). The desired fractions were combined, concentrated, treated with 2 N HCl in ethanol (10 mL), and evaporated (in vacuo, 65° C.) to give a glass (0.17 g, 59%): mp>100° C.; LCMS (+APCI) m/z 292 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06696476B2 |
| Source dataset | uspto-grants-2004_02 |
| ORD ID | ord-4e1f158ff04f4a289c5236416f9cf18e |
| Source note | uspto-grants-2004_02 |