Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 86661753 | HCID 86661753 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86661756 | HCID 86661756 | 98.3% |
Reaction Steps
The product (1.0 g) obtained in Step 1 was dissolved in ethyl acetate (10 mL). To the solution, 10% palladium-carbon (300 mg) was added, and the mixture was stirred at 70° C. for 3 hours in a hydrogen atmosphere. After the completion of reaction, the mixture was returned to room temperature, and dichloromethane (5 mL) was added, followed by filtration through celite. The filtrate was concentrated under reduced pressure, and the obtained residue was dissolved in methanol. 10% palladium-carbon (200 mg) was added again thereto, and the mixture was stirred at 70° C. for 16 hours in a hydrogen atmosphere. The mixture was returned to room temperature, and dichloromethane (5 mL) was added, followed by filtration through celite. The filtrate was concentrated under reduced pressure to obtain the compound of interest as a colorless oil (676 mg, 98.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08951997B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-060e9d162baa4a2e9c5897649e997abc |
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| Source note | uspto-grants-2015_02 |
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