化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → [3-Cyclohexyl-2-(cyclohexylimino)-4-oxo-5-thiazolidinylidene]acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium iodide | HCID 66321 | — |
| 反応物 | Methyl [3-cyclohexyl-2-(cyclohexylimino)-4-oxo-5-thiazolidinylidene]acetate | HCID 3967510 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [3-Cyclohexyl-2-(cyclohexylimino)-4-oxo-5-thiazolidinylidene]acetic acid | HCID 54247385 | 67.9% |
反応手順
A mixture of methyl [3-cyclohexyl-2-(cyclohexylimino)-4-oxo-5-thiazolidinylidene]acetate (5.0 g, 14 mmoles) and anhydrous lithium iodide (7.6 g, 57 mmoles) in N,N-dimethylformamide (30 mls) is heated under argon to reflux. After six hours the mixture is cooled, diluted with water, acidified with 4N HCl, and extracted twice with dichloromethane. The combined extracts are washed with brine and dried over MgSO4. The solvent is removed to afford a syrupy residue which evenually crystallizes. Recrystallization from acetonitrile gave the product (3.2 g), mp 189°-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04775677 |
| 出典データセット | uspto-grants-1988_10 |
| ORD ID | ord-62b0d1a1851d45a79744ced82a0f96dc |
| 出典メモ | uspto-grants-1988_10 |