関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,5-Dichloro-3-pyridylamine | HCID 77886 | — |
| 反応物 | 1,1'-Thiocarbonyldi-2(1H)-pyridone | HCID 853162 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3,5-Dichloro-2-isothiocyanatopyridine | HCID 23340445 | 88.3% |
反応手順
To 3,5-dichloropyridin-2-amine (0.36 g, 2.209 mmol) in dichloromethane (25 mL) was added 1,1′-thiocarbonyldipyridin-2(1H)-one (0.523 g, 2.253 mmol). The reaction was stirred at 40° C. for 3 hours. The reaction was cooled to room temperature and the crude was purified by chromatography (Biotage: 25-100% ethyl acetate/hexane) to yield to yield 3,5-dichloro-2-isothiocyanatopyridine (0.4 g, 1.951 mmol, 88% yield). 1H NMR (500 MHz, DMSO-D6) δ ppm 8.50 (t, J=2.59 Hz, 1 H), 8.45 (t, J=2.59 Hz, 1 H). MS (LC/MS) R.T.=2.07; [M+H]+=204.8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07863291B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-3c18546b68874bb7ba4a02a5fef5411a |
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| 出典メモ | uspto-grants-2011_01 |
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