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Monomethyl-5-nitroisophthalate → 3-Amino-5-(methoxycarbonyl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Monomethyl-5-nitroisophthalate | HCID 6931682 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Amino-5-(methoxycarbonyl)benzoic acid | HCID 13557643 | — |
反応手順
To 2.75 g of mono-methyl 5-nitroisophthalate (5-(methoxycarbonyl)-3-nitrobenzoic acid), compound 67, dissolved in 30 mL of THF was added 100 mg of 10% palladium on carbon. The reaction was placed in a Parr hydrogenator under a H2 atmosphere of 45 psi and shaken for 16 hr. The solid palladium catalyst was removed by vacuum filtration through celite and 5 mL of 1N HCl in diethyl ether was added to the filtrate. After sitting for 12 hr, the solid was collected by vacuum filtration and was washed with ethyl acetate. This provided 1.82 g of the desired product. The product was identified by 1H NMR and mass spectroscopy and purity was assessed by RP-HPLC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06653321B1 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-a83ddcf2e0354fd7ac022d81a00c447c |
| 出典メモ | uspto-grants-2003_11 |