HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzylethanolamine → 2-[Benzyl({3-chloro-5-[cyclobutyl(methyl)amino]pyrazin-2-yl}methyl)amino]ethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzylethanolamine | HCID 4348 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 86648997 | HCID 86648997 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2-[Benzyl({3-chloro-5-[cyclobutyl(methyl)amino]pyrazin-2-yl}methyl)amino]ethanol | HCID 86648998 | 92.6% |
Reaction Steps
Sodium triacetoxyborohydride (0.71 g) was added to a solution of 3-chloro-5-[cyclobutyl(methyl)amino]pyrazine-2-carbaldehyde (0.50 g), N-benzylethanolamine (0.40 g) and acetic acid (0.38 mL) in acetonitrile (8 mL), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was basified with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The aqueous layer was extracted again with ethyl acetate. The combined organic layer was washed with water and saturated brine, dried over magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (solvent gradient: 10→60% ethyl acetate/hexane) to give the title compound (0.74 g, 92%) as a pale-yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08314088B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-29d7cb38da0243e7b7438e0c923b8a16 |
| Source note | uspto-grants-2012_11 |