関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-(Isopropylamino)ethanol | HCID 7994 | — |
| 反応物 | N-(2-fluoro-5-nitrophenyl)methanesulfonamide | HCID 4416401 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2'-[2-(Isopropylamino)ethoxy]-5'-nitromethanesulfonanilide | HCID 18368289 | 88.4% |
反応手順
2-(Isopropylamino)ethanol (24,0 g) solution in dimethylformamide (70 ml) was added with potassium tert-butoxide (21.9 g) in an ice bathing. After being stirred for 1 hour at room temperature, the reaction mixture was cooled down to 5° C. and added drop-wise with 2′-fluoro-5′-nitromethanesulfonanilide (21.8 g) in dimethylformamide (30 ml). After being stirred for 3 hours at room temperature, the reaction mixture was added into ethyl acetate (500 ml) and solids formed were collected by filtration and washed with ethyl acetate (100 ml). Solids obtained were dissolved into water (200 ml) and the solution was adjusted to pH=7 with 2N HCl . Resultant crystals were collected by filtration, washed with water, and dried under vacuum to obtain 2′-[2-(isopropylamino)ethoxy]-5′-nitromethanesulfonanilide (26.1 g) as white crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06300368B1 |
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| 出典データセット | uspto-grants-2001_10 |
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| ORD ID | ord-986b22ad33be4b148ecbe07641450da2 |
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| 出典メモ | uspto-grants-2001_10 |
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