HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Imatinib amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 24897293 | HCID 24897293 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | Imatinib amine | HCID 9965429 | — |
Reaction Steps
In an autoclave, 5 g 6-chloro-N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine amine, 0.5 g palladium on charcoal 5% wet with 50% water, 50 mL ethanol and 5 mL triethylamine is charged. The mixture is hydrogenated at 5 bars and room temperature for 40 hours. Once completed the conversion, the catalyst is filtered off and the filtrates is concentrated in vacuum. The residue is taken again with isopropyl acetate and an aqueous carbonate solution. The layers are separated, and the organic layer is concentrated, yielding, upon drying, 3 g of product with 85% HPLC purity (A %), which is identified through LC-MS and 1H-NMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168787B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-019bce1397884201807a1b32f14ae4e1 |
| Source note | uspto-grants-2012_05 |