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Acetic Anhydride → 9-Acetoxy-4,4-dimethyl-7-(1,2-dimethylheptyl)-1,2,3,4-tetrahydrocyclopenta[c][l] benzopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Cyclopenta(c)(1)benzopyran-9-ol, 1,2,3,4-tetrahydro-4,4-dimethyl-7-(1,2-dimethylheptyl)- | HCID 215348 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 9-Acetoxy-4,4-dimethyl-7-(1,2-dimethylheptyl)-1,2,3,4-tetrahydrocyclopenta[c][l] benzopyran | HCID 21853910 | — |
反応手順
A solution of 4,4-dimethyl-9-hydroxy-7-(1,2-dimethylheptyl)-1,2,3,4-tetrahydrocyclopenta[ c][l]benzopyran (6.85 g., 0.02 mole) and acetic anhydride (3.06 g., 0.03 mole) in 20 ml. of pyridine was warmed over a steam bath with stirring for 2 hours. The reaction mixture was allowed to cool to room temperature and the pyridine was removed by evaporation under reduced pressure. Water was added to the residue and this aqueous mixture was extracted with three portions of ether. The ether extracts were washed several times with water, 6N HCl, again with water, and dried over Na2SO4. Solvent evaporation in vacuo left 7.59 g. (99%) of crude acetate. The ir and nmr were in agreement with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04051152 |
| 出典データセット | uspto-grants-1977_09 |
| ORD ID | ord-cd0a699458314b2ba21c7bbbcea18164 |
| 出典メモ | uspto-grants-1977_09 |