HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl acetate hexane → HCID 23152957, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Reactant | HCID 23153357 | HCID 23153357 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23152957 | HCID 23152957 | 71.1% |
Reaction Steps
Benzyl N-{4-[6-(pyrrolidin-1-ylcarbonyl)aminopyrimidin-4-ylamino]phenyl]carbamate (210 mg) was dissolved in tetrahydrofuran (5 ml)-methanol (5 ml), and then 10% palladium carbon (200 mg) was added thereto under a nitrogen atmosphere, followed by replacing with hydrogen inside the system and stirring for 5 hrs. After replacing with nitrogen inside the system, the reaction mixture was filtered to remove the catalyst, which was washed with tetrahydrofuran and ethanol in this order. The filtrate was concentrated under a reduced pressure to give a residue, to which hexane-ethyl acetate was added to precipitate crystals. The crystals were filtered, and dried under aeration to provide the titled compound (103 mg, 71%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07531532B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-8da402d8b0ad45f084ea9f9f0afb38a5 |
| Source note | uspto-grants-2009_05 |