HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86641034, compound → HCID 24986794, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86641034 | HCID 86641034 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | HCID 24986794 | HCID 24986794 | 80% |
Reaction Steps
The compound (1.0 eq.) obtained in Step 1 was dissolved in a mixed solvent of ethylalcohol/methylene chloride (3:1, 0.01˜0.1 M) to which Pd(OH)2 (500 massa) was then added. The resulting reaction mixture was stirred for 5˜8 hrs at room temperature under 1 atm of hydrogen gas. After the filtration of the metal catalyst through a Celite pad, the reaction mixture was washed with a solution of ethylalcohol/methylene:chloride (3:1). After two rounds of centrifugation at 1000 rpm for 10 min, the supernatant was concentrated and dried in a vacuum. The concentrate was precipitated in a mixed solvent of hexane/ethyl acetate (1:1) to afford the object compound as a white wax solid (24 mg, 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08883746B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-bd712470620f4f0ba317dc6b2524cd65 |
| Source note | uspto-grants-2014_11 |