HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 4-[2-(3-Bromo-4-chloro-benzoylamino)-phenyl]-butyric acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methyl 4-(2-aminophenyl)butanoate | HCID 237256 | — |
| Reactant | 3-Bromo-4-chlorobenzoyl chloride | HCID 20229730 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[2-(3-Bromo-4-chloro-benzoylamino)-phenyl]-butyric acid methyl ester | HCID 68602147 | 101.9% |
Reaction Steps
To 3-bromo-4-chloro-benzoyl chloride (1.09 g, 4.3 mmol) in DCM (30 mL) cooled with an ice bath, was added 4-(2-amino-phenyl)-butyric acid methyl ester (0.85 g, 4.4 mmol), followed by addition of diisopropylethylamine (1 mL, 5.6 mmol) slowly. Upon the completion of the addition, ice bath was removed and the mixture was stirred at room temperature for 12 hrs. The mixture was further diluted with DCM, washed with saturated NaHCO3, 1N HCl, brine and dried over Na2SO4 and concentrated to yield 4-[2-(3-bromo-4-chloro-benzoylamino)-phenyl]-butyric acid methyl ester (1.8 g). MS [M+H]+: 411.7; tR=2.45 min. (method 1)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422310B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-68351de091e246ce87bde63f435e25f8 |
| Source note | uspto-grants-2016_08 |