HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67231452, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1-(Methylsulfonyl)piperazine | HCID 709161 | — |
| Reactant | HCID 67232390 | HCID 67232390 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 67231452 | HCID 67231452 | 49.4% |
Reaction Steps
A solution of the compound (0.31 g) obtained in Example 419 and 1-(methylsulfonyl)piperazine (0.14 g) in 1-methyl-2-pyrrolidone (5 mL) was stirred at 110° C. for 24 hr and at 135° C. for 14 hr. The reaction mixture was poured into water, and extracted twice with ethyl acetate. The extract was washed with saturated aqueous ammonium chloride solution and saturated brine, dried and concentrated. The residue was purified by silica gel column chromatography (solvent gradient; 75→100% ethyl acetate/hexane) to give the title compound (0.16 g, 48%) as a pale-yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592454B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-23e40220e906471fb1520ba40d5041de |
| Source note | uspto-grants-2013_11 |