化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → Ethyl 4-[14-(trimethylsilyl)tetradecylamino]hippurate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Glycine ethyl ester | HCID 12176 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 4-[14-(Trimethylsilyl)tetradecylamino]benzoyl chloride hydrochloride | HCID 20198230 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl 4-[14-(trimethylsilyl)tetradecylamino]hippurate | HCID 20198242 | — |
反応手順
A solution of 20 g. 4-[14-(trimethylsilyl)tetradecylamino]benzoyl chloride hydrochloride in 100 ml. dioxane is added to 4.9 g. freshly prepared ethyl glycinate in 300 ml. of methylene chloride containing 1 g. of 4-(dimethylamino)pyridine and 10 ml. of triethylamine. After 16 hours at room temperature the reaction is refluxed for 2 hours, cooled and filtered. The mother liquor is extracted with water and 10% hydrochloric acid. The solution is dried and concentrated in vacuo to an amber liquid. A sample is chromatographed on silica, appropriate fractions are pooled and evaporated to yield a solid which is recrystallized to a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04670421 |
| 出典データセット | uspto-grants-1987_06 |
| ORD ID | ord-6b5996995f4e4a588ac5b7b2229113ed |
| 出典メモ | uspto-grants-1987_06 |