참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Acetophenone | HCID 7410 | — |
| 반응물 | Triethyl phosphonoacetate | HCID 13345 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethyl (2E)-3-phenyl-2-butenoate | HCID 5354836 | 128.9% |
반응 단계
A mixture of 10 g (0.25 mol) of sodium hydride and tetrahydrofuran is heated to 50° C., followed by dropwise addition over 30 minutes of a solution of 48 ml (0.19 mol) of ethyl diethylphosphonoacetate in 80 ml of tetrahydrofuran. A solution of 28.4 g (0.24 mol) of acetophenone in 60 ml of tetrahydrofuran is added dropwise at 0° C. and the mixture is stirred for 16 hours at 25° C. 250 ml of saturated sodium chloride solution are added at 0° C. and the resulting mixture is extracted with ether. The organic phase is dried (Na2SO4) and the solvents are evaporated off under reduced pressure. The 46.6 g of product obtained are purified by flash chromatography (90/10 cyclohexane/diisopropyl ether) (29 g; 63%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737176B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-e57508df4c494718b30ab937cbf2203a |
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| 출처 메모 | uspto-grants-2010_06 |
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