関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | N,N-Dimethyl-4-nitro-2-sulfamoylbenzamide | HCID 22066001 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 触媒 | Sodium Molybdate | HCID 61424 | — |
| 生成物 | N,N-Dimethyl-2-aminosulfonyl-4-formamidobenzamide | HCID 15240549 | — |
反応手順
A suspension of 40 g N,N-Dimethyl 2-aminosulfonyl-4-nitrobenzamide (VIII), sodium molybdate (0.08 g) and Pd/C (3 g, 5%, 50% water) in formic acid (200 ml) was hydrogenated at 50° C. and 40 bar for 7 hours. The catalyst was then filtered and washed with formic acid (20 ml). The filtrate was concentrated in vacuo and ethyl acetate (200 ml) added. After stirring for 2 hours at 20° C. the product was filtered, the filtrate concentrated and re-filtered. The combined solids were washed with ethyl acetate (20 ml) and dries at 50° C./50 mbar. Yield: 35.3 g (=84.3%), 94.1% w/w, mp.: 192-193° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07781611B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-2859279ccf80494dbc0d185f567de2f3 |
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| 出典メモ | uspto-grants-2010_08 |
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