HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → Benzoic acid, 4-(bromomethyl)-2-ethoxy-, ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Benzoic acid, 2-ethoxy-4-methyl-, ethyl ester | HCID 11816602 | — |
| Solvent | 2-Methylbenzotrifluoride | HCID 2775324 | — |
| Product | Benzoic acid, 4-(bromomethyl)-2-ethoxy-, ethyl ester | HCID 10589339 | 30.4% |
Reaction Steps
To a solution of ethyl 2-ethoxy-4-methylbenzoate (100 mg, 0.481 mmol) in 2 mL of trifluoromethyl toluene was added NBS (94 mg, 0.529 mmol) and AIBN (10 mg) in portions. The mixture was heated to reflux and stirred for 24 h. The reaction mixture was concentrated, diluted with 10 mL of EA, washed with 5 mL of 4 N NaOH, 5 mL of brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford ethyl 4-(bromomethyl)-2-ethoxybenzoate as brown oil (42 mg, 30%), which was used for the next step directly.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09283229B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-7f89417a31c04851bca2a2df7247c45c |
| Source note | uspto-grants-2016_03 |