HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → HCID 10403337, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Diisopropylcarbodiimide | HCID 12734 | — |
| Reactant | HCID 10334336 | HCID 10334336 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10403337 | HCID 10403337 | — |
Reaction Steps
A solution of 5-amino-4-[(4-chlorophenyl)amino]-6-(ethylamino)pyrimidine-2-carbonitrile (0.41 g, prepared using the method of example 20) in acetonitrile (5 ml) was added to a stirred solution of FMOC-NCS (0.44 g) in acetonitrile (10 ml) at 0° C. After 1 h, diisopropylcarbodiimide (0.252 g) was added, the mixture heated under reflux for 4 h, cooled, piperazine (0.1 g) added and stirred at room temperature for 3 h. The solvent was removed under reduced pressure and the residue partitioned between ethyl acetate and brine, the organics dried (MgSO4) and evaporated under reduced pressure. The solid was purified by chromatography on silica eluting with 2-4% methanol in dichloromethane. Yield 0.12 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07439240B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-96c20059431d4fa9a0592d8450f46033 |
| Source note | uspto-grants-2008_10 |