HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Methyl 2-[(3-chloropropyl)amino]-4-methoxy-3-nitrobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-[(3-Chloropropyl)amino]-4-methoxy-3-nitrobenzoic acid | HCID 68739420 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Methyl 2-[(3-chloropropyl)amino]-4-methoxy-3-nitrobenzoate | HCID 68736083 | 86.3% |
Reaction Steps
To a mixture of 2-[(3-chloropropyl)amino]-4-methoxy-3-nitrobenzoic acid (1.77 g, 6.13 mmol) and potassium carbonate (847 mg, 6.13 mmol) in N,N-dimethylformamide (18 mL) was added iodomethane (0.38 mL, 6.10 mmol) at room temperature. After stirring at room temperature for 14 hr, water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water (×5) and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with a 10-50% ethyl acetate/n-hexane gradient mixture to give the title compound (1.60 g, 5.29 mmol, 86%) as a yellow amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785460B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-07764ce268874889933cfeb044b00014 |
| Source note | uspto-grants-2014_07 |