참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Lithium Chloride | HCID 433294 | — |
| 반응물 | Methyl 4-p-tolylsulfonyl-4-methyl-3-dimethoxymethylpentanoate | HCID 12850320 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | trans 4-(2-Chloro-prop-2-yl)-5-hydroxy-tetrahydrofuran-2-one | HCID 12882418 | 109.4% |
반응 단계
A mixture of 1 g of the product of Example 2, 25 ml of ether and 1 g of dry lithium chloride was stirred under a current of gaseous hydrogen chloride at -30° C. for 2 hours and then at 0° C. for 2 hours after which the current of gaseous hydrogen chloride was stopped. The mixture was stirred at room temperature for 48 hours and after 54 hours of contact, the mixture was poured into iced water. The mixture was extracted with benzene and the organic phase was dried and evaporated to dryness under reduced pressure. The 1.1 g of residue was chromatographed over silica gel and was eluted with a 1-1 benzene-ethyl acetate mixture to obtain 545 mg of dl trans 4-(2-chloro-prop-2-yl)-5-hydroxy-tetrahydrofuran-2-one in the form of crystals melting at 80° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04382037 |
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| 출처 데이터셋 | uspto-grants-1983_05 |
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| ORD ID | ord-f478c52a4cc440aa81e8c7f737a8accb |
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| 출처 메모 | uspto-grants-1983_05 |
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