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Nitroxyl → N-[4-[2-(dibutylamino)-1-hydroxyethyl]phenyl]methanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitroxyl | HCID 945 | — |
| 反応物 | N-[4-[2-(Dibutylamino)-1-oxoethyl]phenyl]methanesulfonamide | HCID 19873466 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-[4-[2-(dibutylamino)-1-hydroxyethyl]phenyl]methanesulfonamide | HCID 19873459 | — |
反応手順
A mixture of 0.46 g (1.35 mmol) of the ketoamine free base, N-[4-[2-(Dibutylamino)-1-oxoethyl]phenyl]methanesulfonamide, 0.15 g of 10% palladium on carbon catalyst and 150 ml of absolute EtOH is placed on a Parr hydrogenator and shaken under an hydrogen atmosphere for 18.5 hrs. The catalyst is removed by filtration and the filtrate is concentrated in vacuo. The residue is chromatographed on a 100 ml silica gel column (elution with 3% MeOH:CH2Cl2 containing 0.3% NH4OH) and fractions are collected. The title compound is recrystallized from Et2O:pet. ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05155268 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-515880a395ab4aaf96785221c93ee8f6 |
| 出典メモ | uspto-grants-1992_10 |