Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Anthranilic Acid | HCID 227 | — |
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Bentranil | HCID 13926 | — |
Reaction Steps
Anthranilic acid (1.0 g, 7.29 mmol) was dissolved in pyridine (10 mL), benzoyl chloride (1.13 g, 8.02 mmol) was slowly added on an ice bath, and stirred at 50° C. overnight. The solvent was distilled off under reduced pressure, the residue was dissolved in dry methylene chloride (20 mL), oxalyl chloride (925 mg, 7.29 mmol) and a catalytic amount of dimethylformamide were added on an ice bath, and stirred at room temperature for 4 hours. Saturated sodium hydrogen carbonate aqueous solution was added, the mixture was extracted with methylene chloride, and the organic phase was dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, the residue was washed by diethyl ether/heptane, and the target substance (1.13 g, 69%) was obtained as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268842B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-4fdf7ff2c6b2412e8485ef3b2cb7093f |
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| Source note | uspto-grants-2012_09 |
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