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Triethylamine → m-PEG4-succinimidyl carbonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Tetraethylene glycol monomethyl ether | HCID 90263 | — |
| 反応物 | Di(succinimido) carbonate | HCID 676246 | — |
| 反応物 | Ethylacetate methanol | HCID 21584119 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | m-PEG4-succinimidyl carbonate | HCID 59659904 | 28% |
反応手順
Tetraethylene glycol monomethyl ether (1.0 g, 4.8 mmol) and N,N′-disuccinimidyl carbonate (1.48 g, 5.8 mmol) were dissolved in acetonitrile (10 mL). Then triethylamine (1.0 mL, 7.2 mmol) was added and the reaction stirred overnight at room temperature. Crude reaction was evaporated to dryness, dissolved in sat. NaHCO3 (30 mL), washed ethyl acetate (2×30 mL), dried MgSO4, and evaporated to dryness. Column chromatography (Silica, ethyl acetate/MeOH, 20:1) afforded 1 a clear oil (0.462 g, 28% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09102758B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-b3e9539dee4241a190a4ffc0e7def378 |
| 出典メモ | uspto-grants-2015_08 |