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P-Phenylenediamine → N1-((2-(Pyridin-2-ylamino)thiazol-5-yl)methyl)benzene-1,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | P-Phenylenediamine | HCID 7814 | — |
| 反応物 | Triethylsilane | HCID 12052 | — |
| 反応物 | 2-(Pyridin-2-ylamino)thiazole-5-carbaldehyde | HCID 22019058 | — |
| 溶媒 | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| 生成物 | N1-((2-(Pyridin-2-ylamino)thiazol-5-yl)methyl)benzene-1,4-diamine | HCID 59852979 | — |
反応手順
A solution of 2-(pyridine-2-ylamino)-thiazole-5-carbaldehyde (0.10 g, 0.49 mmol, WO2004/001059), benzene-1,4-diamine (0.105 g, 0.97 mmol) and triethylsilane (0.19 mL, 1.2 mmol) in CH2Cl2-TFA (3:1, 4 mL) was stirred at ambient temperature for 4 h. The reaction mixture was concentrated in vacuo and the residue partitioned between CH2Cl2 and saturated aqueous NaHCO3 solution. The organic phase was washed with saturated aqueous NaHCO3 solution, brine, dried (MgSO4) and concentrated in vacuo. The crude product which contained the title compound along with the starting aldehyde and benzene-1,4-diamine was carried on directly into the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07989477B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-34030195678644c2b21e26d6c1505759 |
| 出典メモ | uspto-grants-2011_08 |