HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67352936, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methyl Anthranilate | HCID 8635 | — |
| Reactant | 4-Bromo-3-methylbenzoyl chloride | HCID 7021534 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67352936 | HCID 67352936 | 86% |
Reaction Steps
To 2-amino-benzoic acid methyl ester (3.1 g) in dichloromethane (31 mL) was slowly added 4-bromo-3-methyl-benzoyl chloride [21900-25-4] (4.8 g) and triethylamine (3.1 mL). The reaction mixture was then stirred at room temperature for 1 hour. After such time, the reaction mixture was further diluted with dichloromethane (50 mL) and washed with water. The combined aqueous phase was further extracted with dichloromethane. All combined organic phases were then dried over sodium sulfate and concentrated in vacuo. The residue was then recrystallised from ethanol to give 2-(4-bromo-3-methyl-benzoylamino)-benzoic acid methyl ester (6.14 g) as white crystals, m.p.=123° C. MS (m/e): 348.3 (M+H+, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989657B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-ea2e344171e548e18370f1612686ea6a |
| Source note | uspto-grants-2011_08 |