HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 131730969, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Azane;hydrate | HCID 12896473 | — |
| Reactant | HCID 131730968 | HCID 131730968 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 131730969 | HCID 131730969 | 57.6% |
Reaction Steps
60 mg of 6-({4-[4-(2-aminoethyl)piperazin-1-yl]phenyl}amino)-4-[(3,5-difluorobenzyl)amino]pyridine-3-carboxyamide (the compound of Example 248) was suspended in 6 mL of chloroform, to which, under ice cooling, 20 mg of pyridine and 17 mg of methanesulfonyl chloride were added, and stirred at the same temperature for 20 minutes. To the reaction mixture, ammonia water was added, extracted with chloroform, the extract was washed with saturated saline, and dried on anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel thin layer chromatography (chloroform:methanol=5:1), recrystallized from chloroform-methanol-ether to obtain 40 mg (57%) of the title compound as a slight yellow crystalline powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575153B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-92fafa26e51345819cf3fdf07141d072 |
| Source note | uspto-grants-2013_11 |