HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 30425Generated: October 26, 2026
1,2-Dichloroethane → 6-Oxo-n-(2-piperidinoethyl)-3-(phenylamino)-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide
https://huagongshe.com/reaction/30425
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | N-(2-Aminoethyl)piperidine | HCID 33944 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Ammonium 6-oxo-3-(phenylamino)-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxylate | HCID 66971000 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-Oxo-n-(2-piperidinoethyl)-3-(phenylamino)-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide | HCID 68457272 | 21.2% |
Reaction Steps
To a suspension of the compound of Example 14 (90 mg, 0.23 mmol) in DCM (2 mL) was added EDC (60 mg, 0.30 mmol) and HOBT (41 mg, 0.30 mmol) and the mixture stirred at r.t. for 15 minutes. A solution 1-(2-aminoethyl)piperidine (45 mg, 0.35 mmol) in DCM (0.5 mL) was added and the reaction stirred at r.t. for 18 h. The reaction mixture was diluted with DCM (10 mL), washed with water (2×5 mL), dried (MgSO4) and concentrated in vacuo. The crude product was purified by chromatography on silica (0-20% THF in DCM) to give the title compound as an off-white solid (23 mg). δH (CDCl3) 8.61 (1H, s), 7.61-7.43 (3H, m), 7.40-7.27 (2H, m), 7.25-7.13 (3H, m), 7.00-6.89 (3H, m), 6.50 (1H, bs), 6.33 (1H, d, J 9.7 Hz), 3.43-3.25 (2H, m), 2.47-2.32 (2H, m), 2.31-2.11 (4H, m), 1.50-1.40 (4H, m), 1.39-1.25 (2H, m). LCMS (ES+) RT 2.40 minutes, 473 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07423047B2 |
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| Source dataset | uspto-grants-2008_09 |
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| ORD ID | ord-564c538e2f854295a05549fcac003bec |
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| Source note | uspto-grants-2008_09 |
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