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Ethyl Acetate → 5-amino-2-methyl-N-(pyrimidin-5-yl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-methyl-5-nitro-N-(pyrimidin-5-yl)benzamide | HCID 24823255 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-amino-2-methyl-N-(pyrimidin-5-yl)benzamide | HCID 24824047 | — |
反応手順
A 2L high-pressure vessel was charged with Palladium 10% on carbon wet (50% water) and EtOAc (50 mL). 2-methyl-5-nitro-N-(pyrimidin-5-yl)benzamide 45 (18.79 g) was dissolved in methanol (400 mL) and added to the previous mixture. The reaction vessel was pressurized to 30 psi of H2 and mechanically stirred until the hydrogen intake stopped. The reduction of the nitro group was complete by LCMS and the mixture was filtered off through paper and glass paper. The crude 5-amino-2-methyl-N-(pyrimidin-5-yl)benzamide 46 was obtained as a yellow solid and used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08492404B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-0464d5cdc18f482d940e198df9ce7402 |
| 出典メモ | uspto-grants-2013_07 |