참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl (2E)-3-methyl-4-oxo-2-butenoate | HCID 6009828 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | HCID 86603586 | HCID 86603586 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 86603585 | HCID 86603585 | — |
반응 단계
3 g (8.4 mmol) of ethyl [2-(2-isobutoxy-5-methoxyphenyl)-2-oxoethyl]-phosphonate dissolved in 20 ml of tetrahydrofuran are added dropwise to a suspension of 1.41 g (12.6 mmol) of potassium tert-butoxide in 30 ml of tetrahydrofuran, heated to 50° C. Heating is continued for 20 minutes at 50° C., the mixture is then cooled to 0° C. and 1.8 g (12.6 mmol) of ethyl 3-methyl-4-oxocrotonate dissolved in 20 ml of tetrahydrofuran are added dropwise. The reaction mixture is then stirred for 72 hours at 25° C. Water is added and the resulting mixture is extracted with ether. After drying (Na2SO4), the solvent is evaporated off and the residue is purified by flash chromatography (dichloromethane) (2.58 g of yellow oil; 89%).
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-a324b16e61e64ab7b1a0c8ce6fe558cf |
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| 출처 메모 | uspto-grants-2010_06 |
|---|