HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butylamine → N-tert-butyl-6-chloropyridazine-3-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butylamine | HCID 6385 | — |
| Reactant | Bis(2-oxo-3-oxazolidinyl)phosphinic chloride | HCID 152842 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 6-chloropyridazine-3-carboxylic Acid | HCID 6415762 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-tert-butyl-6-chloropyridazine-3-carboxamide | HCID 12059835 | 49.3% |
Reaction Steps
To a solution of 6-chloro-3-pyridazinecarboxylic acid (0.12 g, 0.76 mmol) in methylene chloride (15 ml) were added t-butylamine (0.21 ml, 2.0 mmol) and N,N-bis(2-oxo-3-oxazolidinyl)phosphinic chloride (0.24 g, 0.93 mmol), and stirred overnight. The reaction mixture was added to saturated aqueous NaHCO3 and extracted three times with ethyl acetate. The combined organic layers were washed with brine and dried over Na2SO4. The solvent was evaporated and the residue was purified by silica gel chromatography (hexane/ethyl acetate=2/1) to give the title compound (0.080 g; 49%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936736B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-692f00977b6245a681161be3d1ac57e8 |
| Source note | uspto-grants-2005_08 |