関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Maleimide | HCID 10935 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(Methoxycarbonyl)maleimide | HCID 580610 | 55% |
反応手順
Methylchloroformate (4.4 mL, 56.7 mmol, 1 eq) was added to a solution of maleimide (5.5 g, 56.7 mmol, 1 eq) and NMM (6.2 mL, 56.7 mmol, 1 eq) in 200 mL of EtOAc at 0° C. The suspension was stirred at 0° C. for 30 minutes, filtered and washed with EtOAc. Filtrate and washings were combined and washed with cold water and dried over anhydrous Na2SO4. After filtration and evaporation under vacuum a pink solid was obtained. Purification by column chromatography on silica gel (Hexane-EtOAc, 1:1, v/v) provided the product (4.8 g, 55%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08367065B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-f1acf67d1cd44f2980ceb3ef2322c62b |
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| 出典メモ | uspto-grants-2013_02 |
|---|