HuagongsheHuagongshe Chemistry Print Report · For research reference only
Morpholine → 4-(2-Fluoro-5-nitrobenzyl)morpholine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-(Bromomethyl)-1-fluoro-4-nitrobenzene | HCID 10353967 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(2-Fluoro-5-nitrobenzyl)morpholine | HCID 86713637 | 81% |
Reaction Steps
A −20° C. mixture of DIEA (552 mg, 4.27 mmol) and morpholine (242 mg, 2.78 mmol) in THF (5 mL) was treated drop-wise with a solution of 2-(bromomethyl)-1-fluoro-4-nitrobenzene (500 mg, 2.137 mmol) in THF (5 mL) and stirred overnight as the cooling bath expired. The mixture was treated with EtOAc, washed with water, then brine, dried over Na2SO4 and concentrated to dryness to afford 4-(2-fluoro-5-nitrobenzyl)morpholine (414 mg, 81% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.30 (dd, J=6.2, 3.0 Hz, 1H), 8.21 (ddd, J=9.0, 4.4, 3.0 Hz, 1H), 7.48 (t, J=9.1 Hz, 1H), 3.61 (s, 2H), 3.56 (t, J=4.6 Hz, 4H), 2.40 (t, J=4.4 Hz, 4H); MS (ESI) m/z: 241.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461179B1 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-524475b8ccd24aa1a2a6d5fcff832581 |
| Source note | uspto-grants-2013_06 |