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6-Hydroxy-3-methyl-4-vinyl-phthalic Acid Dimethyl Ester → 4-Ethyl-6-hydroxy-3-methyl-phthalic Acid Dimethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-Hydroxy-3-methyl-4-vinyl-phthalic Acid Dimethyl Ester | HCID 59794498 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Ethyl-6-hydroxy-3-methyl-phthalic Acid Dimethyl Ester | HCID 59794477 | 88.4% |
反応手順
6-Hydroxy-3-methyl-4-vinyl-phthalic acid dimethyl ester (1.27 g, 5.11 mmol) was dissolved in benzene (10 mL) and EtOAc (10 mL). Tristriphenylphosphine rhodium chloride (150 mg) was added and the reaction was placed under an atmosphere of hydrogen. Stirring at room temperature was continued. After 14 hrs, the solvents were removed in vacuo and the crude material was purified by silica gel chromatography to provide 1.14 g (88%) of the desired product as an off-white solid. 1H NMR (300 MHz, CDCl3): δ=1.19 (t, J=7.8 Hz, 3H), 2.10 (s, 3H), 2.60 (q, J=7.8 Hz, 2H), 3.89 (s, 6H), 6.87 (s, 1H), 10.79 (s, 1H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871785B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-3ec88630a0b14892b121578b8e337c5d |
| 出典メモ | uspto-grants-2014_10 |