HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzylamine → HCID 117892046, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,4-Dichloro-5-nitropyridine | HCID 12275765 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 117892046 | HCID 117892046 | 66% |
Reaction Steps
To a solution of 2,4-dichloro-5-nitro-pyridine E-2.1″ (5.000 g; 25.908 mmol) in NMP are added DIPEA (8.372 ml, 51.817 mmol) and benzylamine (3.054 ml, 28.499 mmol). The mixture is stirred for 1 h at RT. 1-Methylpiperazine (3.172 ml; 28.499 mmol) is then added and the mixture is stirred at 50° C. overnight. The residue is loaded onto isolute, split into 5 portions and purified using the basic preparatory reversed phase chromatography (method: prep. HPLC1). Product containing fractions are combined and freeze-dried (yield: 66%, 5.619 g; 17.163 mmol)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296748B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-afe407f9d6974f9094ddbe26116574bf |
| Source note | uspto-grants-2016_03 |