참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trimethyl orthoformate | HCID 9005 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 반응물 | Ethyl 3-formyl-4-methoxybenzoate | HCID 638670 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Ethyl 3-dimethoxymethyl-4-methoxybenzoate | HCID 23141411 | 97% |
반응 단계
Ethyl 3-formyl-4-methoxybenzoate (500 mg) obtained in step C of Example 1-2-1 was dissolved in 10 mL of methanol. Trimethyl orthoformate (263 μL) and 41 mg of p-toluenesulfonic acid monohydrate were added to the solution, and then the mixture was heated for 2 hours under reflux. After the reaction solution was cooled, 5 mL of a saturated aqueous solution of sodium bicarbonate was added, and the resulting mixture was concentrated under reduced pressure. The residue was diluted with ethyl acetate, washed with purified water and then with a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate. The anhydrous sodium sulfate was separated by filtration, whereafter the filtrate was concentrated under reduced pressure. The residue was dried under reduced pressure to obtain 596 mg (97%) of ethyl 3-dimethoxymethyl-4-methoxybenzoate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08063046B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_11 |
|---|
| ORD ID | ord-48dbf8b5698148bba2bc54c8f0b52c3a |
|---|
| 출처 메모 | uspto-grants-2011_11 |
|---|