Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,4-Difluorobenzoyl chloride | HCID 588081 | — |
| Reactant | HCID 15481711 | HCID 15481711 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 53949972 | HCID 53949972 | 47% |
Reaction Steps
To a mixture of compound 2 (674 mg, 2 mmol) and triethylamine (0.55 ml, 4 mmol) in tetrahydrofuran (10 ml) was added dropwise 2,4-difluorobezoyl chloride (440 mg, 2.5 mmol) in 5 ml tetrahydrofuran at 0° C. The reaction mixture was stirred at 0° C. for 30 minutes and at room temperature for 18 h. The solvent was removed under reduced pressure, the residue was dissolved in dichloromethane (50 ml). The organic phase was washed with brine, dried over sodium sulphate. The solvent was removed under reduced pressure and the resulting product was purified on a column of silica gel (EtOAc/hexane, 9:1) to give the title compound as colorless prisms (448 mg, 47%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06153616 |
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| Source dataset | uspto-grants-2000_11 |
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| ORD ID | ord-cb967cfd0bf3459aa236e3155e1bf0f6 |
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| Source note | uspto-grants-2000_11 |
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