HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Bromobenzaldehyde → 4-(4-Bromo-benzylamino)-2-hydroxy-benzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Bromobenzaldehyde | HCID 70741 | — |
| Reactant | Methyl p-aminosalicylate | HCID 77787 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-(4-Bromo-benzylamino)-2-hydroxy-benzoic acid methyl ester | HCID 58685863 | 58% |
Reaction Steps
To a solution of 4-amino-2-hydroxy benzoic acid methyl ester (836 mg; 5 mmol) and 4-bromobenzaldehyde (926 mg; 5 mmol) in 1 M HOAc in 1,2-dichloroethane (5 mL) was added at once NaBH(OAc)3 (1.49 g; 7 mmol) and the reaction mixture was stirred at room temperature overnight. Water (25 mL) was added and the inhomogeneous mixture was neutralized using solid NaHCO3. The organic layer was isolated, dried, evaporated to dryness and recrystallised from isopropyl ether/dichloromethane/heptane to yield 970 mg (58%) of a yellow solid. NMR and GC-MS in accordance with structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07741352B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-27627b1c3a684507b64c67ddba27ff91 |
| Source note | uspto-grants-2010_06 |