HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl Bromide → HCID 46179255, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 86639351 | HCID 86639351 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 46179255 | HCID 46179255 | 30.4% |
Reaction Steps
Methyl 2-oxo-2-piperazinylethyl (2E)but-2-ene-1,4-dioate hydrochloride (14) (0.50 g, 1.71 mmol) was reacted at ca. 0° C. with benzyl bromide (BnBr) (0.243 mL, 0.35 g, 2.05 mmol) and diisopropylethylamine (DIEA) (1.00 mL, 0.74 g, 5.76 mmol) in dichloromethane (DCM) followed by warming to room temperature. After aqueous work-up, the crude product was purified by mass-guided preparative HPLC to afford 0.18 g (27% yield) of the title compound (15) as a white solid. 1H NMR (CDCl3, 400 MHz): δ 7.08-7.01 (m, 5H), 6.72-6.71 (m, 2H), 4.60 (s, 2H), 3.58-3.57 (s, 3H), 3.23-3.19 (br S, 2H), 3.30 (s, 2H), 3.1.19-3.11 (br S, 2H), 2.23 (br S, 4H); MS (ESI) m/z 347.13 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785443B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-1e6b6579ea08407c94ee29cc8470d1d4 |
| Source note | uspto-grants-2014_07 |