HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Reactant | N-(6-chloro-2-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide | HCID 19353544 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide | HCID 17774522 | 43.8% |
Reaction Conditions
| Temperature | 140 °C |
|---|
Reaction Steps
0.36 g (0.0011 mol) of N-(6-chloro-2-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide was dissolved in 10 ml of ethanol, treated with 1.2 g (0.018 mol) of methylamine hydrochloride and 4.0 ml (0.029 mol) of triethylamine and stirred in an autoclave at 140° C. for 17 hours. The mixture was freed completely from solvent, the residue was partitioned in ethyl acetate/water, the insoluble constituents were filtered off under suction and extracted. The extract and the solid were combined and recrystallized from methanol/diethyl ether. There was obtained 0.15 g (43%) of N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide as white crystals; m.p. 261-263° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05939451 |
| Source dataset | uspto-grants-1999_08 |
| ORD ID | ord-3a1dde55a88d4522ae1768c2385e0592 |
| Source note | uspto-grants-1999_08 |