HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 178426674, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 2-Dimethylamino-6-methylisonicotinonitrile | HCID 66933468 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178426674 | HCID 178426674 | 33.7% |
Reaction Steps
To an ice-cooled solution of potassium tert.-butylate (1.71 g, 15.2 mmol) in methanol (50 mL), hydroxylamine hydrochloride (905 mg, 13.02 mmol) is added. The suspension is stirred for 30 min before 2-dimethylamino-6-methyl-isonicotinonitrile (699 mg, 4.34 mmol) is added. The mixture is refluxed for 2 h before it is evaporated. The residue is dissolved in a small amount of water and separated by MPLC on RP-C18-silica gel to give 2-dimethylamino-N-hydroxy-6-methyl-isonicotinamidine (284 mg) as a brownish resin; LC-MS: tR=0.60 min, [M+1]+=195.42.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598208B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-e9da8ceb1cf44d81a8a28a652e2f5a74 |
| Source note | uspto-grants-2013_12 |