HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → 4-Amino-N-methylpyridine-3-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Aminonicotinic acid | HCID 319979 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Amino-N-methylpyridine-3-carboxamide | HCID 58835255 | — |
Reaction Steps
To the mixture of 4-aminonicotinic acid (691 mg, 5.0 mmol), methylamine hydrogen chloride (410 mg, 1.2 eq), EDC (1.15 g, 1.2 eq), HOBt (810 mg, 1.2 eq) in DMF (20 mL) was added DIEA (3.0 mL, 3.0 eq). The mixture was stirred at room temperature overnight. It was concentrated and dissolved in EtOAc. It was washed with saturated NaHCO3 solution. It was concentrated and purified by silica gel with chromatography (0%˜20% MeOH/DCM) to obtain the desired product 4-amino-N-methylnicotinamide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501763B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-eddce89a73b345a6a420f7694bcb8717 |
| Source note | uspto-grants-2013_08 |