참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | p-(Dimethoxymethyl)anisole | HCID 75140 | — |
| 반응물 | Dimethylolpropionic acid | HCID 78501 | — |
| 촉매 | p-Toluenesulfonic acid | HCID 6101 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 2-(4-Methoxyphenyl)-5-methyl-1,3-dioxane-5-carboxylic acid | HCID 585147 | 74.4% |
반응 단계
2,2-bis(hydroxymethyl)propionic acid (10 g) and anisaldehyde dimethyl acetal (20.4 g) were added to acetone (50 ml) at 20-25° C. p-Toluenesulfonic acid (0.51 g) was added to the reaction mixture and stirred at 20-25° C. for 5 hours. The mixture was then cooled to 0-5° C. and stirred for 1 hour. The slurry was filtered and the solid was washed with chilled (0-5° C.) acetone (10 ml). The solid was dried under vacuum at 45-50° C. for 4 hour. The solid was added to toluene (150 ml) and the resulting mixture was heated at 65-70° C. for 2 hours. The mixture was then cooled to 5-10° C. and stirred for 30 minutes. The slurry was filtered and the solid was washed with toluene (10 ml) followed by drying under vacuum at 30-35° C. for 4 hours to obtain title compound (14.0 g, 74.4%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08524893B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-ce5852ba11a14809924815902305fdbd |
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| 출처 메모 | uspto-grants-2013_09 |
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