HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 68522763, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 91551434 | HCID 91551434 | — |
| Product | HCID 68522763 | HCID 68522763 | — |
Reaction Steps
A solution of 93.1 mg (0.2 mmol) of tert-butyl[(1R)-3-oxo-3-(2-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylhydrazino)-1-(2,4,5-trifluorobenzyl)propyl]carbamate in 10 mL of glacial acetic acid was stirred at reflux under nitrogen for 40 h. The cooled solution was concentrated, and the residue was partitioned between 5 mL of ethyl acetate and 3 mL of saturated sodium carbonate aqueous solution. The organic phase was dried over magnesium sulfate, filtered, and concentrated to dryness. The residue was purified by preparative thin-layer chromatography on silica gel (92.5:7.5 dichloromethane:methanol), giving the title compound as a white solid, mp 233-235° C. LC-MS 390 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07625888B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-1a5af77e1d0f4e0892091b411822a056 |
| Source note | uspto-grants-2009_12 |