HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59754298, compound → HCID 59754261, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59754298 | HCID 59754298 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | HCID 178418361 | HCID 178418361 | — |
| Product | HCID 59754261 | HCID 59754261 | 26.7% |
Reaction Steps
Compound 46E (80 mg, 0.20 mmol) was dissolved in MeOH (5 mL) and hydrogenated at 1 atmosphere of hydrogen for 24 h in the presence of 20 mg Pd(OH)2. The reaction was then filtered, concentrated under reduced pressure, and subsequently purified by silica gel flash chromatography eluting with a gradient of 5%-10% MeOH in CH2Cl2 to give the title compound (16 mg) as a white solid. HPLC: 98% at 0.79 min (retention time) (Conditions: YMC S5 C18 (4.6×50 mm); Eluted with 0% to 100% B, 8 min gradient, 3 min hold. (A=90% H2O-10% MeCN-0.1% TFA and B=10% H2O-90% MeCN-0.1% TFA); Flow rate at 2.5 mL/min UV detection at 220 nm). LC/MS m/z 300 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07772267B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-b7c5934b4fc84e728922c30eac334477 |
| Source note | uspto-grants-2010_08 |