化工社化工社 化学情報印刷レポート · 研究参考用
Heptane → 1,2,2-Trimethyl-1,3-cyclopentanedicarboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Heptane | HCID 8900 | — |
| 反応物 | 1,2,2-Trimethyl-1,3-cyclopentanedicarboxylic acid | HCID 21491 | — |
| 反応物 | Dimethyl Fumarate | HCID 637568 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1,2,2-Trimethyl-1,3-cyclopentanedicarboxylic acid | HCID 21491 | — |
| 生成物 | Dimethyl Fumarate | HCID 637568 | — |
| 生成物 | Dimethyl fumarate (+)-camphoric acid | HCID 117762171 | — |
反応手順
Cocrystals of dimethyl fumarate and (+)-camphoric acid were prepared as follows. 150 mg of dimethyl fumarate and 225 mg of (+)-camphoric acid were dissolved in 3 ml of ethyl acetate with stirring and gentle heating. The clear solution was cooled to room temperature, and 9 ml of heptane were added. The unstirred solution was allowed to stand for 24 hours. The starting concentrations of dimethyl fumarate and (+)-camphoric acid were chosen such that the thermodynamically stable solid phase at equilibrium is the cocrystal of dimethyl fumarate and (+)-camphoric acid. The crystalline material that formed was isolated by vacuum filtration, and dried to yield the dimethyl fumarate: (+)-camphoric acid (1:16, by NMR) cocrystal form 1 (112 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09421182B2 |
| 出典データセット | uspto-grants-2016_08 |
| ORD ID | ord-c10884af3f2948cd802d5f3e298534c0 |
| 出典メモ | uspto-grants-2016_08 |