HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Pyridinamine, N-methyl- → HCID 112686069, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Pyridinamine, N-methyl- | HCID 20727 | — |
| Reactant | Chlorosulfamic acid | HCID 24499 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 112686069 | HCID 112686069 | — |
Reaction Steps
To a stirred solution of NaH (60%) (0.112 g, 2.78 mmol) in THF (6 ml), N-methylpyridin-2-amine (prepared by N-methylation of 2-aminopyridine) (0.3 g, 2.78 mmol) in THF (2 ml) was added and stirred for 1 h. To this a solution of Sulfamoyl chloride (0.32 g, 2.78 mmol) in THF (1 ml) was added and stirred for 2 h at RT. Reaction mass was quenched with methanol (0.6 ml) at ice cold condition and concentrated to dryness to get crude which was purified using neutral alumina column, eluent ethyl acetate in n-Hexane 0 to 85% to afford N-methyl-N-(pyridin-2-yl)sulfamide as off white solid (0.12 g, 23% yield)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394305B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-dd9243b3c3de4b0ab56d915a9c1c27a7 |
| Source note | uspto-grants-2016_07 |