HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → 5-(4-Methylpiperazin-1-yl)pyridin-2-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1-Methyl-4-(6-nitropyridin-3-yl)piperazine | HCID 51711484 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Water ethanol | HCID 19096565 | — |
| Product | 5-(4-Methylpiperazin-1-yl)pyridin-2-amine | HCID 22329833 | 60% |
Reaction Steps
The suspension of 1-methyl-4-(6-nitropyridin-3-yl)piperazine (5 g, 22.5 mmol), NH4Cl (12 g, 225 mmol), and Fe (5 g, 5 mmol) was stirred in EtOH/H2O (1:1) (100 mL) at 80° C. for 3 h. TLC showed starting material 1-methyl-4-(6-nitropyridin-3-yl)piperazine disappeared. After filtration on a pad of Celite, the solvent was removed under vacuum. EA and brine were added into the mixture and the organic layer was separated, dried over Na2SO4 and concentrated at reduced pressure to give 2.5 g of 5-(4-methylpiperazin-1-yl)pyridin-2-amine (yield 60%). LCMS: (M+H)+ 193
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08618107B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-5880db29c803426a8d08e62a73b5d696 |
| Source note | uspto-grants-2013_12 |