HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59165959, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phthalic Anhydride | HCID 6811 | — |
| Reactant | Methyl 6-aminonicotinate | HCID 737487 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 59165959 | HCID 59165959 | 60% |
Reaction Steps
A solution of 6-aminonicotinic acid methyl ester (1.1 g, 7.2 mmol) and phthalic anhydride (1.2 g, 7.9 mmol) in anhydrous toluene was heated at reflux overnight in a Dean-Stark apparatus until no more water was collected. The reaction mixture was concentrated under vacuum. The residue was dissolved in ethyl acetate (50 mL) and was washed with brine and water. The organic layer was dried over anhydrous Na2SO4 and concentrated under vacuum to give 6-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-nicotinic acid methyl ester (1.2 g, 60%), which was directly used in the next step without further purification. 1H NMR (300 MHz, d-DMSO) δ 9.12 (d, J=1.5 Hz, 1H), 8.52 (dd, J=2.1, 8.4 Hz, 1H), 8.03-7.92 (m, 4H), 7.72 (d, J=7.8 Hz, 1H), 3.91 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08324207B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-e482342beeef4668a34b6dd81c125818 |
| Source note | uspto-grants-2012_12 |