HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24765378, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | HCID 68833307 | HCID 68833307 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 24765378 | HCID 24765378 | 71% |
Reaction Steps
A solution of lithium borohydride (2.0 M in THF, 0.34 mL) was added to a solution of (2S,3S)-2-(4-chloro-benzenesulfonylamino)-4,4,4-trifluoro-3-methyl-butyric acid ethyl ester (126 mg, 0.34 mmol) in THF (5 mL) and stirred for 12 h. Careful addition of 2N HCl (aq) was performed until pH<2. Organic solvent was removed in vacuo. The aqueous layer was extracted with EtOAc (2×20 mL) and organic layers were combined and washed with brine. The organic layer was dried over Na2SO4 and solvent removed in vacuo. The crude solid was purified by flash chromatography (20% EtOAc/hexanes) to provide a white solid (80 mg) in 71 % yield. Mass Spectrum (−ESI): 330.0 [M−H]−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07550629B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-0eb29a96498c407f88be342289a208e1 |
| Source note | uspto-grants-2009_06 |