HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68934618, compound → HCID 57531737, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68934618 | HCID 68934618 | — |
| Reactant | n-[3-Chloro-4-(4-methylpiperazin-1-yl)phenyl]guanidine | HCID 178480750 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 57531737 | HCID 57531737 | 33% |
Reaction Steps
A solution of ethyl 6-(hydroxymethylene)-1,5,5-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate (400 mg, 1.44 mmol) and N-[3-chloro-4-(4-methyl-piperazin-1-yl)-phenyl]-guanidine (424 mg, 1.58 mmol) in anhydrous dimethylformamide (5 mL) was heated at 100° C. for 3 hours. After cooling, the reaction mixture was poured into brine (50 mL) and extracted with ethyl acetate (50 mL×2). The extracts were collected, dried on Na2SO4 and evaporated to dryness. The crude material was purified by flash chromatography on silica gel eluted with dichloromethane/methanol 9:1 to give the pure title compound (240 mg, 33% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08541429B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-a3806bfdbac44df39cadcfd46cc4aef2 |
| Source note | uspto-grants-2013_09 |