関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyl-4-methoxyaniline | HCID 7610 | — |
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Methoxy-2-methylphenyl isothiocyanate | HCID 142405 | 79.2% |
反応手順
To a solution of 4-methoxy-2-methylaniline (2.51 mL, 19.7 mmol) and saturated aqueous sodium hydrogen carbonate (13.5 mL) in tetrahydrofuran (13.5 mL) was added thiophosgene (1.50 mL, 19.7 mmol), and the mixture was stirred at 0° C. for 30 min. The reaction mixture was 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 purified by flash column chromatography on silica gel eluting with a 0-10% ethyl acetate/n-hexane gradient mixture. The desired fractions were concentrated in vacuo to give the title compound as a colorless oil (2.80 g, 15.6 mmol, 79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08785460B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-349a4690aa764bf4918ec2da70817490 |
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| 出典メモ | uspto-grants-2014_07 |
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