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Triethylamine → N,N'-Bis(benzyloxycarbonyl)-3-[carboxymethoxyacetyl]-3-azapentane-1,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,4-Dioxane-2,6-dione | HCID 78232 | — |
| 反応物 | N,N''-Di-Z-diethylenetriamine | HCID 4367374 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N,N'-Bis(benzyloxycarbonyl)-3-[carboxymethoxyacetyl]-3-azapentane-1,5-diamine | HCID 54008985 | — |
反応手順
37.14 g (100 mmol) of the bis(benzyloxycarbonylaminoethyl)-amine described in Example 1a is dissolved in DMF, mixed in an ice bath with 17.4 g (150 mmol) of diglycolic anhydride (Janssen Chimica) and 21 ml (150 mmol) of triethylamine and then stirred overnight at room temperature. The solution is concentrated by evaporation in a vacuum, the residue is taken up in ethyl acetate and shaken out with diluted hydrochloric acid. The organic phase is dried with sodium sulfate and after filtration from drying agent, it is crystallized by adding hexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06248306B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-47f7d99797424acb961b5b03aec76798 |
| 出典メモ | uspto-grants-2001_06 |