Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | HCID 46849446 | HCID 46849446 | — |
| Product | HCID 70817703 | HCID 70817703 | 50.4% |
Reaction Steps
In a thick-walled glass vial equipped with a magnetic stir bar was placed methyl(E)-4-(2,4,5-trifluorophenyl)-but-2-enoate (IIa) (0.5 mmol, 115 mg) and reaction system was slowly heated to 60° C. under intensive stirring. Afterwards benzylamine (0.6 mmol; 66 mL) was slowly added to (IIa) and such reaction system was vigorously stirred (800 rpm) at 70° C. for 12 hours. The reaction mixture was than extracted with tert-butyl methyl ether (20 mL), organic phase was washed with brine (20 mL) and dried over anhydrous Na2SO4. After evaporation of organic solvent under reduced pressure we obtained crude product (Ib) (85 mg, 50% yield) which was analyzed and confirmed with 1H and 13C NMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09359385B2 |
|---|
| Source dataset | uspto-grants-2016_06 |
|---|
| ORD ID | ord-d40d8dbc92244a4a9201a1effbe194b2 |
|---|
| Source note | uspto-grants-2016_06 |
|---|