HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → HCID 9971655, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | HCID 10243527 | HCID 10243527 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 9971655 | HCID 9971655 | 63.1% |
Reaction Steps
The process is performed as in Example 75, starting with 500 mg of 2-chloro-N-(6-chloro-1H-indazol-3-yl)acetamide, 15 cm3 of acetonitrile and 528 mg of piperazine. The reaction medium is refluxed for 1 hour and then concentrated to dryness under reduced pressure (2 kPa; 50° C.); the crude product is purified by chromatography under an argon pressure of 50 kPa, on a column of silica gel (particle size 40-60 μm; diameter 2.5 cm), eluting with a methylene chloride/methanol/aqueous ammonia mixture (90/10/1 by volume). The fractions containing the expected product are combined, concentrated under reduced pressure and then dried (90 Pa; 45° C.) to give 380 mg of N-(6-chloro-1H-indazol-3-yl)-1-piperazineacetamide in the form of a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06949579B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-12c80e95dee84e2d9812cfa246ee9f82 |
| Source note | uspto-grants-2005_09 |