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Carbon Dioxide → beta-Phenylisovaleric acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Neophyl chloride | HCID 68191 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | beta-Phenylisovaleric acid | HCID 13890 | — |
反応手順
Magnesium (4,86 g, 0.2 mol, 50-150 mesh), neophylchloride (0.2 g) and tetrahydrofurane(10 ml) were placed in a flask under an atmosphere of argon. A Grignard reaction was then started with 1,2-dibromoethane (0.2 ml). Neophylchloride (35,47 g, 0.2 mol) dissolved in MTBE (50 ml) was then added at reflux over a period of 50 minutes. After stirring for 2½ h at the same temperature, the reaction mixture was diluted with MTBE and dried CO2 was introduced above the surface at a temperature of 35° C. (ice cooling). The mixture was then acidified with HCl and extracted with MTBE. GC revealed the presence of 2,5-dimethyl-2,5-diphenyl-hexane and phenylisobutyric in a ratio of 54:46.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07538243B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-8f474afbc12f4e07bfccb7a52cd11650 |
| 出典メモ | uspto-grants-2009_05 |