化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3.4,5.6-Tetrahydrophthalimidomethyl dispiro(2.0.4.1)nonane-9-Carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | N-(Hydroxymethyl)-3,4,5,6-tetrahydrophthalimide | HCID 78597 | — |
| 反応物 | Dispiro(2.0.4.1)nonan-9-carboxylic acid | HCID 22767648 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3.4,5.6-Tetrahydrophthalimidomethyl dispiro(2.0.4.1)nonane-9-Carboxylate | HCID 22767655 | — |
反応手順
Dispiro(2.0.4.1)nonan-9-carboxylic acid (0.66g) was converted to the corresponding acid chloride by refluxing with thionyl chloride (1ml) in benzene (20 ml) for 1 hour. The acid chloride, N-hydroxymethyl-3,4,5,6-tetrahydrophthalimide (0.7g) and triethylamine (0.5g) were then stirred together in ether (50 ml) for 6 hours. After removal of solvent under reduced pressure the residue was purified by chromatography on silica gel using dichloromethane as eluent. The required product was obtained as an oil R.I. nD18 1.5318.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04118510 |
| 出典データセット | uspto-grants-1978_10 |
| ORD ID | ord-aaf3ae2a005040e89a8cd44fc2b3e927 |
| 出典メモ | uspto-grants-1978_10 |