HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9953741, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 12035491 | HCID 12035491 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9953741 | HCID 9953741 | 72% |
Reaction Steps
To a stirred solution of the product of Example 9 (25 mg, 0.05 mmol), in THF (2 mL), under nitrogen, was added a solution of lithium aluminum hydride (1M in THF, 0.25 mL, 0.25 mmol). The mixture was stirred for 30min at room temperature. Ethyl acetate was added, followed by water, and then acidified with 1N HCl. The whole mixture was applied to a Varian SCX cartridge, and washed in turn with 1N HCl, water, acetone, MeOH, and MeOH/CH2Cl2 (1:1). The product was then eluted with MeOH/CH2Cl2/NH4OH (49:49:2). Evaporation of the eluent gave the title compound (15 mg, 72%). Mp >300° C.; MS(ES) 417, 419 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06770639B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-8b9df7be33194024a90dac612d840e9f |
| Source note | uspto-grants-2004_08 |