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Acetic Acid → 2,6,6-Trimethylfulvene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 1-Methyl-1,3-cyclopentadiene | HCID 66775 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2,6,6-Trimethylfulvene | HCID 14363282 | 92.5% |
反応手順
To 130 ml of dehydrated methanol, 22.6 g (283 mmol) of methylcyclopentadiene and 8.50 ml (116 mmol) of acetone were added, then 14.5 ml (174 mmol) of pyrrolidine was dropwise added at 0° C., and the mixture was reacted at room temperature for one night. Then, 10 ml (180 mmol) of acetic acid was added at 0° C. The mixture was diluted with ether and water and then subjected to extraction. Then, the organic phase was separated, washed with water and dried over anhydrous magnesium sulfate to obtain 12.9 g of a brown liquid. The analyzed values are given below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07449533B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-02e1cd6f9c1b4900b49a714d7d59086e |
| 出典メモ | uspto-grants-2008_11 |