참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,4,5-Trimethoxybenzoic acid | HCID 10276 | — |
| 반응물 | Aluminum chloride, hexahydrate | HCID 24564 | — |
| 반응물 | Sodium Bromide | HCID 253881 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Hydroxy-4,5-dimethoxybenzoic acid | HCID 11564650 | 73.2% |
반응 단계
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%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08841461B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-e0f61f8f6ad84412b7b220996880d35e |
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| 출처 메모 | uspto-grants-2014_09 |
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