HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1775967Generated: October 27, 2026
Potassium Phosphate, Tribasic → 9-(2-(3,4-difluorophenyl)prop-1-enyl)-2,6-dimethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole
https://huagongshe.com/reaction/1775967
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | L-Proline | HCID 145742 | — |
| Reactant | 2,3,4,9-Tetrahydro-2,6-dimethyl-1H-pyrido[3,4-b]indole | HCID 757133 | — |
| Reactant | 4-(1-Bromoprop-1-en-2-yl)-1,2-difluorobenzene | HCID 86635504 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 9-(2-(3,4-difluorophenyl)prop-1-enyl)-2,6-dimethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole | HCID 66911695 | 58.5% |
Reaction Steps
2,6-dimethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole (72 mg, 0.359 mmol) was dissolved in DMF (5 mL). To this solution was added CuI (8 mg, 0.035 mmol), L-proline (9 mg, 0.086 mmol), K3PO4 (183 mg, 0.862 mmol). The reaction mixture was stirred for 10 min at room temperature followed by addition of 4-(1-bromoprop-1-en-2-yl)-1,2-difluorobenzene (100 mg, 0.431 mmol). The reaction mixture was heated at 80° C. overnight. Solvent was evaporated under reduced pressure; the residue was diluted with brine and extracted with ethyl acetate. Organic layer was dried over Na2SO4, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography to obtain 74 mg of 9-(2-(3,4-difluorophenyl)prop-1-enyl)-2,6-dimethyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole. 1H NMR (DMSO) OXALATE SALT 7.80 (m, 1H), 7.50 (m, 2H), 7.30 (s, 1H), 7.20 (s, 1H), 7.15 (d, 1H), 7.0 (d, 1H), 4.22 (m, 2H), 3.40 (m, 2H), 2.90 (m, 2H), 2.82 (s, 3H), 2.40 (s, 3H), 1.90 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09260429B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-fac13d7973704661a5f0490922396dfd |
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| Source note | uspto-grants-2016_02 |
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