関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-Thiocarbonyldi-2(1H)-pyridone | HCID 853162 | — |
| 反応物 | 6-Amino-2,4-dimethyl-3-pyridinecarbonitrile | HCID 3793299 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Isothiocyanato-2,4-dimethylnicotinonitrile | HCID 18316201 | 790% |
反応手順
To 6-amino-2,4-dimethylnicotinonitrile (0.14 g, 0.95 mmol) in dichloromethane (20 mL) was added 1,1′-thiocarbonyldipyridin-2(1H)-one (0.23 g, 0.1 mmol). The reaction was stirred at 40° C. for 3 hours. The reaction was cooled to room temperature. The crude was purified by chromatography (Biotage: 25-100% ethyl acetate/hexane) to yield 6-isothiocyanato-2,4-dimethylnicotinonitrile (0.15 g, 0.79 mmol, 83% yield). 1H NMR (500 MHz, DMSO-D6) δ ppm 7.37 (s, 1 H), 2.63 (s, 3 H). MS (LC/MS) R.T.=2.40; [M+H]+=190.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 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-f2287e7c01f74480b5b13980987f86e4 |
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| 出典メモ | uspto-grants-2011_01 |
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