HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzylamine → HCID 10800431, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10800431 | HCID 10800431 | 87.3% |
Reaction Steps
A solution of 23.9 g(16.9 mL, 0.15mol) of 3,4-difluoronitrobenzene and 29.1 g(39.2 mL, 0.23 mol) of N,N-diisopropylethylamine in 285 mL acetonitrile was treated with 19.3 g(19.7 mL, 0.18 mol) of benzylamine, followed by warming at reflux for 5 h. The mixture was concentrated in vacuo and the residue was dissolved in 200 mL ethyl acetate, followed by extraction with water (3×50 mL). Drying (Na2SO4) and concentration in vacuo afforded a yellow solid, which was recrystallized from hot ethyl acetate-hexane to afford 32.25 g(87%) of the title compound as yellow-orange needles, mp 97.5-99° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06124334 |
| Source dataset | uspto-grants-2000_09 |
| ORD ID | ord-f4d8ae103f0443b3940b2fb270e6a79e |
| Source note | uspto-grants-2000_09 |