참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 2',4',6'-Trihydroxyacetophenone | HCID 68073 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 생성물 | 1-[2-Hydroxy-4,6-bis(methoxymethoxy)phenyl]ethanone | HCID 10879697 | 41.4% |
반응 단계
In 200 ml of anhydrous tetrahydrofuran were dissolved 30 g of 2',4',6'-trihydroxyacetophenone and 115.0 g of N,N-diisopropylethylamine, and 50.2 g of chloromethyl methyl ether was gradually added to the solution under ice cooling over a period of 20 minutes and the reaction mixture was stirred under ice cooling for 1 hour and at room temperature for 4 hours to effect reaction. After the reaction, the reaction mixture was extracted with 3 l of ether, and the ether layer was washed with water (500 ml×3 times), shaken with a saturated aqueous solution of sodium chloride (300 ml×2 times), dried with anhydrous sodium sulfate, and filtered. The solvent was removed from the filtrate by distillation and the obtained residue was recrystallized from a mixed solvent of methanol and water to obtain 18.9 g (yield=41.4%) of 2'-hydroxy-4',6'-bis(methoxymethoxy)acetophenone in the form of a colorless prism.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05234951 |
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| 출처 데이터셋 | uspto-grants-1993_08 |
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| ORD ID | ord-3d2d469332b34b23b5b5333bdf6b4cdc |
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| 출처 메모 | uspto-grants-1993_08 |
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