HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Iodopyridine-2,6-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2,6-Diaminopyridine | HCID 8861 | — |
| Reactant | N-Iodosuccinimide | HCID 120273 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | 3-Iodopyridine-2,6-diamine | HCID 476218 | 23% |
Reaction Steps
2,6-Diaminopyridine (100 g) was dissolved in DMSO (400 mL), and N-iodosuccinimide (100 g) was added thereto all at once under stirring at room temperature. The reaction solution was stirred for 10 minutes at room temperature, after which water (3.5 L) was added thereto and the precipitated solids were filtered off. The aqueous layer thus obtained was extracted with ethyl acetate (1.3 L) 3 times. The ethyl acetate layers were combined, and which was concentrated under a reduced pressure, and the residue thus obtained was purified by silica gel chromatography (heptane:ethyl acetate=2:3) to obtain the titled compound (24 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183264B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-19efe85b1e8541f4b78299a256290baf |
| Source note | uspto-grants-2012_05 |