HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → Methyl 5-bromo-3-(ethylamino)-2-methylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetaldehyde | HCID 177 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | Methyl 3-Amino-5-bromo-2-methylbenzoate | HCID 24729181 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | Methyl 5-bromo-3-(ethylamino)-2-methylbenzoate | HCID 70872675 | 55% |
Reaction Steps
To a stirred solution of methyl 3-amino-5-bromo-2-methylbenzoate (1.0 g, 4.09 mmol) and acetaldehyde (180 mg, 4.09 mmol) in dichloroethane (10 mL), acetic acid (1.47 g, 24.58 mmol) was added and reaction stirred at room temperature for 30 minutes. Then sodium triacetoxyborohydride (2.6 g, 12.29 mmol) was added at 0° C., allowed to attain room temperature and stirring continued for 2 h. On completion, reaction mixture was diluted with dichloromethane, washed with water, saturated aqueous sodium bicarbonate solution and dried over sodium sulphate. Removal of the solvent under reduced pressure followed by column chromatographic purification afforded the desired compound (600 mg, 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765732B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-c8548c68cf424bb1b6ef5e06a32a40f3 |
| Source note | uspto-grants-2014_07 |