HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → HCID 20711242, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Ethyl 2-(3,4-difluorophenyl)acetate | HCID 11241070 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 20711242 | HCID 20711242 | — |
Reaction Steps
A mixture of ethyl 2-(3,4-difluorophenyl)acetate (1.20 g, 5.99 mmol), N-bromosuccinimide (1.17 g, 6.59 mmol), and 2,2′-azobis(isobutyronitrile) (0.148 g, 0.899 mmol) in CCl4 (20 mL) was gradually heated to reflux and stirred at this temperature overnight. The solvent was removed in vacuum. The residue was purified by flash column chromatography (100% hexanes for 5 minutes, then 0 to 5% of EtOAc in hexanes over 23 minutes). The desired product was obtained as a colorless oil (1.14 g, 68%). 1H NMR (300 MHz, CDCl3) δ 1.31 (d, J=6.0 Hz, 3H), 4.17-4.35 (m, 2H), 5.27 (s, 1H), 7.11-7.20 (m, 1H), 7.24-7.30 (m, 1H), 7.42-7.52 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07514566B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-454728e1eac648a59cb985a3cdf28ec3 |
| Source note | uspto-grants-2009_04 |