HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 178430158, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Reactant | HCID 178430160 | HCID 178430160 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178430158 | HCID 178430158 | 68.9% |
Reaction Steps
To compound 3E (8.0 mg, 0.0190 mmol) in THF (1 mL) was added a 1 M solution of TBAF in THF (0.190 mL, 0.190 mmol). After stirring at rt for 1.5 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-1 8, 21.2×100 mm, eluting with 40-100% solvent B (A=90% H2O-10% MeOH and B=10% H2O-90% MeOH) over 10 min; Flow rate at 20 mL/min; UV detection at 220 nm) to provide the title compound (4.0 mg) as a white solid. MS: m/z 306 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07625923B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-f94e8c351b3846b3ab02710e5e57e946 |
| Source note | uspto-grants-2009_12 |