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Dimethylformamide dimethyl acetal → N-[3-[3-(dimethylamino)-1-oxo-2-propenyl]phenyl]-N-methyl-methanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | n-(3-Acetyl-phenyl)-n-methyl-methanesulfonamide | HCID 67199578 | — |
| 溶媒 | Ethylacetate methanol | HCID 21584119 | — |
| 生成物 | N-[3-[3-(dimethylamino)-1-oxo-2-propenyl]phenyl]-N-methyl-methanesulfonamide | HCID 67197697 | 88.6% |
反応手順
1.58 g (6.96 mmol) of N-(3-acetyl-phenyl)-N-methyl-methanesulfonamide were dissolved in 15 ml of N,N-dimethylformamide dimethylacetal and the resultant solution was refluxed for 18 hours. The excess of volatile reagent was removed by reduced pressure distillation to yield a crude which was chromatographied over silica gel using a gradient of ethyl acetate/methanol as eluent. 1.12 g of N-[3-[3-(dimethylamino)-1-oxo-2-propenyl]phenyl]-N-methyl methanesulfonamide as a yellowish-white solid were obtained (yield 88.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07947688B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-d716f83265e948189c7995b734f245f3 |
| 出典メモ | uspto-grants-2011_05 |