Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 4-fluoro-5-phenyl-1-(pyridin-3-ylsulfonyl)-1H-pyrrole-3-carbaldehyde | HCID 86630975 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 16045079 | HCID 16045079 | 39% |
Reaction Steps
4-Fluoro-5-phenyl-1-(pyridin-3-ylsulfonyl)-1H-pyrrole-3-carbaldehyde (0.27 g) was dissolved in tetrahydrofuran (10 mL), a 2 mol/L solution (0.8 mL) of methylamine in tetrahydrofuran was added, and the mixture was stirred at room temperature for 2 hr. Sodium borohydride (91 mg) and methanol (7 mL) were added, and the mixture was stirred at the same temperature for further 30 min. The reaction mixture was concentrated under reduced pressure. A saturated aqueous sodium hydrogencarbonate solution was added to the residue, and the mixture was extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (hexane-ethyl acetate=19:1→0:1). The above-mentioned operation was repeated to give the title compound (0.22 g, yield 39%) as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08415368B2 |
|---|
| Source dataset | uspto-grants-2013_04 |
|---|
| ORD ID | ord-80bf2fcdcb1b4477b4d823c469fb2c8d |
|---|
| Source note | uspto-grants-2013_04 |
|---|