참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,4-Dihydroxybenzoic Acid | HCID 1491 | — |
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Benzoic acid, 2,4-dimethoxy-, methyl ester | HCID 137451 | — |
반응 단계
50 g of 2,4-dihydroxybenzoic acid, 269 g of potassium carbonate, 123 mL of dimethyl sulfate, and 500 mL of N,N-dimethylformamide were suspended together, and this suspension was stirred for 6.5 hours at 70 to 80° C. Further, 90 g of potassium carbonate and 61 mL of dimethyl sulfate were added to this suspension, which was stirred for another 4 hours at 110 to 115° C. This reaction mixture was added to a mixture of ethyl acetate and water, and adjusted to pH 2 with 6M hydrochloric acid, and then the organic phase was separated therefrom. After the resultant organic phase was washed with water and a saturated sodium chloride solution successively, the washed phase was dried over anhydrous magnesium sulfate, and the solvent was distilled out under reduced pressure. The resultant residue was purified by silica gel column chromatography [eluent; hexane:ethyl acetate=1:2] to yield 54 g of methyl 2,4-dimethoxybenzoate as yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07772285B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_08 |
|---|
| ORD ID | ord-fb59e1c798564fa39839988088ff206f |
|---|
| 출처 메모 | uspto-grants-2010_08 |
|---|