HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86684770, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Chloro-5-pyridinesulfonyl chloride | HCID 2792792 | — |
| Reactant | HCID 66684920 | HCID 66684920 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86684770 | HCID 86684770 | 94% |
Reaction Steps
To a solution of 3-(2-cyclohexyl-6-oxo-piperazin-1-yl)-5-phenyl-thiophene-2-carboxylic acid (0.80 g, 1.90 mmol, 1.0 equiv) in MeCN (20 mL) at room temperature, was added 6-chloro-pyridine-3-sulfonyl chloride (1.10 g, 5.20 mmol, 2.7 equiv) and followed by NaOH (6.94 mL, 1.5 N solution, 10.4 mmol, 5.5 equiv) dropwise. The mixture was stirred at room temperature for 10 minutes. The mixture was acidified with 3 N HCl (2.5 mL), and then diluted with EtOAc (50 mL). The mixture was washed water (25 mL), brine (25 mL), dried (over Na2SO4), filtered and concentrated to give crude product (1.0 g, 94%) as yellow-green solid. MS: 560 [M−H+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040690B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-3d85445ff5cf40f6bf8fa46a41ba974d |
| Source note | uspto-grants-2015_05 |