関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | 6-Methoxy-4-methylpyridin-3-amine | HCID 243170 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 5-Isothiocyanato-2-methoxy-4-methylpyridine | HCID 86632884 | 59% |
反応手順
Thiophosgene (8.9 mL, 120 mmol) was added dropwise to a stirred mixture of 6-methoxy-4-methylpyridin-3-amine (13.8 g, 99.8 mmol) in tetrahydrofuran (100 mL) and saturated aqueous sodium hydrogen carbonate (150 mL) at 0° C., and the mixture was stirred at 0° C. for 2 hr. The mixture was diluted with saturated aqueous sodium hydrogen carbonate, and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was washed with n-hexane to give the title compound as a colorless powder (10.6 g, 58.8 mmol, 59%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08901141B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-d17bc03c4b95426fba488b1b021ca0ff |
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| 出典メモ | uspto-grants-2014_12 |
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