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1,1'-Dimethyl 2,2'-oxybis(acetate) → 5,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane-3,11-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1'-Dimethyl 2,2'-oxybis(acetate) | HCID 201877 | — |
| 反応物 | 1,5-Diamino-1,5-dibenzyloxymethyl-3-azapentane | HCID 19438519 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane-3,11-dione | HCID 19438510 | — |
反応手順
1,5-Diamino-1,5-dibenzyloxymethyl-3-aza-pentane (0.250 g, 0.73 mmol) (Example 6 (d)) and diglycolic acid dimethyl ester (0.118 g, 0.73 mmol) were dissolved in methanol (20 ml). The mixture was refluxed for 6 days. The solvent was evaporated and the mixture chromatographed on a silica column. 5,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane -3,11-dione was isolated as a yellow oil. Yield 0.273 g (85%). FAB MS: 442(M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05198208 |
| 出典データセット | uspto-grants-1993_03 |
| ORD ID | ord-00f9d8ec1268454f8bf1ce31e3dcf480 |
| 出典メモ | uspto-grants-1993_03 |