HuagongsheHuagongshe Chemistry Print Report · For research reference only
Heptane → 2-Isobutyryl-3-methyl-benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Heptane | HCID 8900 | — |
| Reactant | Isobutyryl chloride | HCID 62325 | — |
| Reactant | 2-Bromo-3-methylbenzoic acid | HCID 2735588 | — |
| Reactant | HCID 178418244 | HCID 178418244 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-Isobutyryl-3-methyl-benzoic acid | HCID 59314181 | 58.4% |
Reaction Steps
The solution of 2-bromo-3-methyl-benzoic acid (1.5 g, 6.98 mmol) in 10 mL THF is treated with 1M Bu2Mg/heptane at −15° C. under argon. After stirring for 30 min, 1.6M n-BuLi/hexane is added dropwise at −15° C. and the mixture is left for 1 hr. Then isobutyryl chloride (2.95 ml, 27.9 mmol) is added dropwise. After another 30 min stirring, the reaction is quenched with 2N HCl aqueous solution (2 ml). After concentration, the residue is purified by HPLC to give a pure product (227) as white solid (840 mg, 58%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08569535B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-836175aee40d4ca8b4f4541a62143c4f |
| Source note | uspto-grants-2013_10 |