HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 16731844, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Reactant | HCID 16731679 | HCID 16731679 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 16731844 | HCID 16731844 | 6.6% |
Reaction Steps
To a solution of 75F (8.20 mg, 0.173 mmol) in THF (2 mL) was added a 1 M THF solution of TBAF (0.120 mL, 0.120 mmol). After stirring at rt for 1 h, saturated aqueous ammonium chloride and EtOAc were added and the layers were separated. The organic layer was washed with brine then dried (MgSO4), filtered and concentrated. The resulting residue was purified via preparative HPLC (YMC ODS C-18, 30×250 mm, eluting with 50-90% solvent B (A=90% H2O-10% MeOH and B=10% H2O-90% MeOH) over 15 min; Flow rate at 20 mL/min; UV detection at 220 nm) to provide the title compound (4.10 mg) as a white solid. MS: m/z 360 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07772267B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-3c608284fde14386911321f77f112268 |
| Source note | uspto-grants-2010_08 |