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1,1'-Thiocarbonyldi-2(1H)-pyridone → 4-Isothiocyanato-6-(methoxymethyl)pyrimidine
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-(Methoxymethyl)-4-pyrimidinamine | HCID 21137644 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Isothiocyanato-6-(methoxymethyl)pyrimidine | HCID 57476558 | 49.3% |
反応手順
To a bright orange solution of 1,1′-thiocarbonyldipyridin-2(1H)-one (0.84 g, 3.59 mmol) was in dichloromethane at ambient temperature was added 6-(methoxymethyl)pyrimidin-4-amine (0.5 g, 3.59 mmol). The orange solution was stirred at ambient temperature for 18 h. The solution was purified by column chromatography (0-40% ethyl acetate/hexanes) to afford 4-isothiocyanato-6-(methoxymethyl)pyrimidine (0.32 g, 1.77 mmol, 49% yield) as a yellow solid. 1H NMR (400 MHz, CDCl3) δ ppm 8.91 (1H, d, J=1.26 Hz), 7.19 (1H, d, J=1.01 Hz), 4.52 (2H, s), 3.49 (3H, s). MS (LC/MS) R.T.=1.39; [M+H]+=182.10.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08309577B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-583f225c27bf46e997f710183d6507e1 |
| 出典メモ | uspto-grants-2012_11 |