Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4-(Aminomethyl)Benzoic Acid | HCID 65526 | — |
| Reactant | 1-Naphthalenesulfonyl chloride | HCID 66560 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 67120728 | HCID 67120728 | — |
Reaction Steps
4 N NaOH solution (30 ml) is added to a suspension of 4-(aminomethyl)benzoic acid (5.01 g, 31.82 mmol) in acetone (100 ml). Toluene (100 ml) is added and the reaction is heated at 40° C. to obtain dissolution. The solution is cooled to 0° C. and treated with 1-naphthalene sulfonyl chloride (12 g, 51.35 mmol) in acetone (100 ml) and the resulting reaction mixture is stirred for 3 hours. The reaction is acidified using citric acid and concentrated in vacuo. The residue is taken up in EtOAc and washed with water. The aqueous layer is back extracted with EtOAc and the combined organic layers are washed with water, brine, dried (Na2SO4) and the solvent removed in vacuo to yield a light brown solid. Trituration with Et2O yields the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09139586B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-25058f6587224fcc9480593e2f3bfe75 |
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| Source note | uspto-grants-2015_09 |
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