関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 3-Ethoxy-2,2-dimethyl-3-oxopropanoic acid | HCID 231754 | — |
| 反応物 | 2-Morpholinoethylamine | HCID 408285 | — |
| 反応物 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 68802054 | HCID 68802054 | — |
反応手順
19 g 2,2-Dimethyl-malonic acid monoethyl ester were weighed into a round-bottomed flask and under N2 atmosphere and room temperature, 200 ml tetrahydrofurane, 15.6 ml 4-(2-Aminoethyl)-morpholine and 32.6 ml N-Methylmorpholine were added. The reaction was stirred and cooled down to 5° C. Then, 43.8 g TBTU were added and the mixture was allowed to stir for another 1.5 hours. Finally the solvent was removed and the residue dissolved in 400 ml dichloromethane. This organic phase was washed two times with 500 ml NaHCO3 solution. The dichloromethane phase was dried then the solvent was evaporated. Purity of the product was judged by gas chromatography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09283186B2 |
|---|
| 出典データセット | uspto-grants-2016_03 |
|---|
| ORD ID | ord-457a9135c9e34ee6b321e781a6b88108 |
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| 出典メモ | uspto-grants-2016_03 |
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