HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 58487350, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| Reactant | Sodium bicarbonate methylene chloride | HCID 23716255 | — |
| Reactant | HCID 58486872 | HCID 58486872 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58487350 | HCID 58487350 | 35.4% |
Reaction Steps
To a solution of 5-(3,3,6-trimethyl-2,3-dihydrobenzo[3,4-b]furan-5-yl)pyrazine-2-ylamine (177) (19 mg, 0.075 mmol) in 1 ml DCM was added 2,6-difluorobenzoyl chloride (19 μl, 2 eq) followed by addition of DIEA (65 μl). The resulting solution was stirred at r.t. for 1 h. The reaction mixture was worked up with aq. NaHCO3/DCM. DCM phase was washed with brine, concentrated to dryness. The residue was dissolved in 1 ml THF/MeOH/H2O (5:4:1) and stirred with 1N NaOH (400 μl) at 60° C. for 1 h before worked up with EA/brine. Prep HPLC purification furnished (2,6-difluorophenyl)-N-[5-(3,3,6-trimethyl(2,3-dihydrobenzo[b]furan-5-yl))pyrazin-2-yl]carboxamide (178) (10.5 mg, yield: 35.4%, purity>95%) as off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980629B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-b0b5fd82697441f9aa22009772d5dd3a |
| Source note | uspto-grants-2015_03 |