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Hydrazine hydrate (1:1) → 4-amino-N-methylbenzene-1-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 4-Nitrobenzenesulfonyl methylamide | HCID 86608755 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-amino-N-methylbenzene-1-sulfonamide | HCID 74368 | — |
反応手順
To a solution of the crude 4-nitrobenzenesulfonyl methylamide prepared above in 45 mL of ethanol, was added a 1 mL slurry of Raney Nickel. Hydrazine monohydrate (18 mmol) was added slowly in several portions. A change in the solution colour from yellow to colourless indicated the reaction was complete. The mixture was stirred for an additional 1 hr. The solids were removed by filtration and the solvent was evaporated. The resulting crude material was purified by flash column chromatography eluting with CH2Cl2:MeOH=10:1 to yield 2.09 g (90% for two steps) of the title compound as a pale orange powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434720B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-2af18a93124e4b66859e501bec395da1 |
| 出典メモ | uspto-grants-2016_09 |