HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → HCID 66680134, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Benzhydrylpiperazine | HCID 70048 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-Chloro-2-((2-chloroacetyl)amino)benzoic acid | HCID 4179825 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66680134 | HCID 66680134 | 11% |
Reaction Steps
1.0 g (4.0 mmol) of 5-chloro-2-[(chloroacetyl)amino]benzoic acid obtained in Example 72-(i), 1.0 g (4.0 mmol) of 1-benzhydrylpiperazine, 1.1 g (8.8 mmol) of N,N-diisopropylethylamine, and 60 mg (0.4 mmol) of sodium iodide were stirred in 5 mL of DMF solution at 80° C. for 3 hours. Thereafter, the solvent was distilled off under reduced pressure, H2O was added to the residue, and solids were collected by filtration and dried. The obtained crude product was separated and purified by silica gel column chromatography, and the resultant was then recrystallized using ethyl acetate/n-hexane, thereby giving 198 mg of the target 5-chloro-2-({[4-(diphenylmethyl)piperazine-1-yl]acetyl}amino)benzoic acid (yield: 11%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785473B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-f5a441c3ef914f4c8480e170a23a89c2 |
| Source note | uspto-grants-2014_07 |