関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Bromo-4,5-dimethoxybenzoic acid | HCID 222963 | — |
| 触媒 | Copper Sulfate | HCID 24462 | — |
| 触媒 | Copper sulfate pentahydrate | HCID 24463 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Hydroxy-4,5-dimethoxybenzoic acid | HCID 11564650 | 99.3% |
反応手順
Water (80 mL) was added to the crude crystals of 2-bromo-4,5-dimethoxybenzoic acid produced in Example 1 (20.0 g) and sodium carbonate (10.1 g). The resultant mixture was stirred under heating at 80° C., and a copper sulfate solution prepared from copper sulfate pentahydrate (1.91 g), water (20 mL), and pyridine (3.1 mL) was added to the mixture. The resultant mixture was further heated and stirred at 90 to 100° C. for one hour. The mixture was cooled to 50° C., and concentrated hydrochloric acid (16.0 g) was added dropwise thereto. After cooling of the mixture, the precipitated crystals were filtrated, and then dried under reduced pressure, to thereby produce crude crystals of 2-hydroxy-4,5-dimethoxybenzoic acid (15.08 g) (yield: 99.3%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09096511B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-a7cb3dd4c9b4463dafab59d1590e826e |
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| 出典メモ | uspto-grants-2015_08 |
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