関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | N-Methyldiethanolamine | HCID 7767 | — |
| 反応物 | Maleic Anhydride | HCID 7923 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Lanthanum sesquioxide | HCID 150906 | — |
| 反応物 | Maleic Acid | HCID 444266 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Maleic acid, disodium salt | HCID 6364608 | — |
反応手順
A disodium maleate solution was prepared by dissolving 19.6 g (0.2 mol) of maleic anhydride in 50 ml of water and by adding the resulting maleic acid solution to 33.3 g of a 48% lye solution (0.4 mol NaOH). During the addition the temperature of the reaction mixture was maintained at 70-90° C. Lanthanum(III)oxide, La2O3, (8.15 g, 0.025 mol) was dissolved in 65% nitric acid (16.8 g, 0.173 mol) and in 12 ml of water and added to the reaction mixture together with N-methyl diethanol-amine (11.9 g, 0.1 mol). The reaction mixture was stirred at 85° C. under a reflux condenser for 70 hours. The reaction mixture was cooled and rendered acidic (pH 1-2) by addition of sulfuric acid. The formed La(III)sulfate precipitate was removed by filtration. The remaining sodium sulfate was precipitated by addition of acetone. After filtration and concentration the remaining solution (7.2 g), which contained water 67.6 w-%, the organic compounds were analyzed as silyl or methyl ester derivatives by means of 13C NMR spectra and by GC-MS (table 1, entry 3, and table 2, entry 3, respectively).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06590120B1 |
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| 出典データセット | uspto-grants-2003_07 |
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| ORD ID | ord-40494070c5294564be03e92a75bc5ebc |
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| 出典メモ | uspto-grants-2003_07 |
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