関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Methylbenzaldehyde | HCID 7725 | — |
| 反応物 | Triethyl 2-phosphonopropionate | HCID 107155 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 2-methyl-3-(4-methylphenyl)-2-propenoate | HCID 68712312 | 98.8% |
反応手順
To dimethylformamide (1802 ml) that had been cooled to −10° C. was added sodium tert-butoxide (528.6 g) and the solution was stirred at −5 to 0° C. for 30 min. Triethyl 2-phosphonopropionate (1310 g) was added dropwise thereto at 10° C. or below. The solution was stirred at 2 to 5° C. for 1 hr, and 4-methylbenzaldehyde (600.8 g) was added dropwise thereto at 10° C. or below and the solution was stirred at room temperature for 1 hr. Water was added thereto and the solution was extracted with toluene. The extract was washed with water and the solvent was distilled off to give the title compound as an oil (1009 g, yield 98.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07420070B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-2eb2a4dd9a0740a3b26f8005a0b593f5 |
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| 出典メモ | uspto-grants-2008_09 |
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