참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Dihydroxyacetone dimer | HCID 4180364 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 2-Propanone, 1,3-bis[(tetrahydro-2H-pyran-2-yl)oxy]- | HCID 11010660 | — |
반응 단계
9 g of 2,5-dihydroxy-1,4-dioxane-2,5-dimethanol were introduced into 60 ml of dioxane and the suspension was taken to about 70° C. for 15 minutes, then taken to ambient temperature. Then, 20 ml of 3,4-dihydro-2H-pyran and 300 mg of monohydrated p-toluene sulfonic acid were added. The temperature was held at about 40° C. and then the reaction medium stood overnight at ambient temperature. It was then poured into a mixture of 300 ml of a saturated solution of sodium bicarbonate +10 ml of triethylamine and extraction was carried out 4 times with methylene chloride. The organic phase was washed with salt water and dried. After purification by passing through silica with ethyl cycloacetate/triethylamine: 8/2 as eluant, 17 g of the expected product (pale yellow syrup) were obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05958936 |
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| 출처 데이터셋 | uspto-grants-1999_09 |
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| ORD ID | ord-5ac8e3a25464461abce1d6f84dbe59d5 |
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| 출처 메모 | uspto-grants-1999_09 |
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