関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-({3-[benzyl(methyl)amino]propyl}amino)-N,N-diisobutyl-3-nitrobenzamide | HCID 69027344 | — |
| 反応物 | Tin tetrachloride dihydrate | HCID 85782573 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-amino-4-({3-[benzyl(methyl)amino]propyl}amino)-N,N-diisobutylbenzamide | HCID 69028792 | 78% |
反応手順
Tin chloride dihydrate (3.58 g, 5eq) is added to a solution of 4-({3-[benzyl(methyl)amino]propyl}amino)-N,N-diisobutyl-3-nitrobenzamide (1.44 g, prepared according to the procedure described for Example A1), in ethyl acetate (40 ml). The mixture is heated under reflux for 7 hours then cooled down to a temperature of approximately 20° C. and poured into a saturated solution of NaHCO3. After decanting and extracting with ethyl acetate, the organic phases are combined, washed with salt water, dried over sodium sulphate and concentrated under reduced pressure at 40° C. Purification by flash chromatography on silica gel (eluent dichloromethane/methanol 95:5) produces the compound in the form of a foam (1.06 g, 78% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07495110B2 |
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| 出典データセット | uspto-grants-2009_02 |
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| ORD ID | ord-264714a6cab04921b7215076ee4f40b8 |
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| 出典メモ | uspto-grants-2009_02 |
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