関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,4,5-Trimethoxybenzoic acid | HCID 10276 | — |
| 反応物 | Aluminum chloride, hexahydrate | HCID 24564 | — |
| 反応物 | Sodium Bromide | HCID 253881 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Hydroxy-4,5-dimethoxybenzoic acid | HCID 11564650 | 73.2% |
反応手順
In 11 mL of dimethylformamide (DMF) were suspended 2.12 g of compound (1a), 4.82 g of AlCl3.6H2O, and 2.06 g of NaBr in a stream of argon, which was then heat stirred at 100° C. for 5 hours. The reaction mixture was allowed to stand to cool, to which 10.4 g of 35% hydrochloric acid was then added dropwise before adding 11 mL of water, followed by heat stirring at 70° C. for one hour. The precipitated crystal was collected by filtration and washed with water. The resultant crystal was dried under reduced pressure at 60° C. to provide 1.45 g of compound (2a) at a yield of 73%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841461B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-e0f61f8f6ad84412b7b220996880d35e |
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| 出典メモ | uspto-grants-2014_09 |
|---|
