関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4-bromo-3-chloro-N-trimethylsilanylmethylthiobenzamide | HCID 86685705 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzimidic acid methyl ester | HCID 66836659 | 76.2% |
反応手順
To a solution of 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzamide (10.40 g, 30.88 mmol) in THF (200 mL) was added methyl iodide (5.77 mL, 13.15 g, 92.7 mmol) and Cs2CO3 (30.19 g, 92.7 mmol) at −5° C. After 1 h at this temperature, the mixture was heated at 40° C. and stirred over night. Water was added and the mixture was extracted three times with MTBE. The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuum. The residue was purified by filtration over a short plug of silica gel to give the title compound (8.25 g), which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653000B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-c293342cb2f44c8c9470e59173be86d6 |
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| 出典メモ | uspto-grants-2014_02 |
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