HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → HCID 58154533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Benzoic acid, 3-methyl-2-nitro-, methyl ester | HCID 79621 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 58154533 | HCID 58154533 | 21.7% |
Reaction Steps
To a mixture of methyl 3-methyl-2-nitrobenzoate (45.0 g, 0.23 mol) and NBS (45.0 g, 0.25 mol) in CCl4 (1500 mL) was added AIBN (1.2 g, 7.3 mmol) portion-wise under reflux. The mixture was refluxed (48 hours), and the solvent was removed in vacuo. The residue was purified by silica gel column chromatography (6% to 10% Ethyl acetate gradient in petroleum ether) to obtain methyl 2-amino-3-(aminomethyl)benzoate (9.0 g, 14% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08685970B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-028e4a4a4a1540e2b7ee8bbec6ed880e |
| Source note | uspto-grants-2014_04 |