HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 70059335, compound → HCID 70059316, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 70059335 | HCID 70059335 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Piperidine | HCID 8082 | — |
| Product | HCID 70059316 | HCID 70059316 | — |
Reaction Steps
The product from Example H (3.90 g, 8.42 mmol) was suspended in 50 mL of 20% piperidine in dichloromethane at room temperature with stirring (2 h). The solution was concentrated under reduced pressure and partitioned between ethyl acetate and water (100 mL each) and separated. The organic layer was washed with 5% sodium bicarbonate (2×50 mL), brine (2×50 mL), dried with magnesium sulfate, filtered and concentrated under reduced pressure to an oil. The oil was purified by silica gel chromatography with ethyl acetate and methanol (3:1). Appropriate fractions were combined and concentrated under reduced pressure to a solid (1.34 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06423689B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-0f3be5abad524da192a7bf844918b70a |
| Source note | uspto-grants-2002_07 |