HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Formylbenzoic acid → 4-[(3,4-Dimethoxyphenylamino)-methyl]-benzoic Acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Formylbenzoic acid | HCID 12088 | — |
| Reactant | Dibutyltin dichloride | HCID 12688 | — |
| Reactant | Phenylsilane | HCID 12752 | — |
| Reactant | 3,4-Dimethoxyaniline | HCID 22770 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 4-[(3,4-Dimethoxyphenylamino)-methyl]-benzoic Acid | HCID 22478880 | 67% |
Reaction Steps
In a 50 ml flask, a mixture of 4-aminoveratrole (1.53 g, 10 mmol), 4-formyl-benzoic acid (1.50 g, 10 mmol), dibutyltin dichloride (304 mg, 1 mmol), phenylsilane (2.47 ml, 20 mmol) in anhydrous THF (10 mL) and DMA (10 ml) was stirred overnight. at room temperature. After solvents removal, the crude residue was dissolved in ethyl acetate (100 ml) and then washed with saturated aqueous solution of NaHCO3 (50 ml×3). The combined aqueous layers were acidified with 6% of NaHSO4 to pH=4. The resulting white suspension was filtrated and then the filter cake was washed with water (5 ml×3). The cake was dried over freeze dryer to afford acid (1.92 g, 67%) white solid product. LRMS=288 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07868204B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-d017c17079b74955a1c8d74d8fe0dc31 |
| Source note | uspto-grants-2011_01 |