참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Diethyl (1,3-Dithian-2-yl)phosphonate | HCID 10869064 | — |
| 반응물 | 4-(4-Phenoxyphenyl)-4-oxobutyrate | HCID 19904354 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl 4-(1,3-dithian-2-ylidene)-4-(4-phenoxyphenyl)-butyrate | HCID 14674064 | 61% |
반응 단계
2-Diethoxyphosphoryl-1,3-dithiane, 2.82 g, was dissolved in 30 ml of tetrahydrofuran and 7 ml of 1.6 mole hexane solution of n-butyl lithium was dropwise added to the solution in an argon flow at -65° C. The mixture was stirred at the same temperature for an hour. Then, a solution of 2.8 g of 4-(4-phenoxyphenyl)-4-oxobutyrate in 10 ml of tetrahydrofuran was dropwise added to the mixture at the same temperature. The reaction mixture was gradually warmed to room temperature overnight. This suspension was poured onto saturated sodium chloride aqueous solution followed by extraction with chloroform. After drying the chloroform phase over magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (chloroform : hexane =1 : 1) to give 2.33 g of the product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05098928 |
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| 출처 데이터셋 | uspto-grants-1992_03 |
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| ORD ID | ord-b0d51a5dd3db444388b54f54bc6a53ad |
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| 출처 메모 | uspto-grants-1992_03 |
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