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Methyl iodide → 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzimidic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-bromo-3-chloro-N-trimethylsilanylmethylthiobenzamide | HCID 86685705 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzimidic acid methyl ester | HCID 66836659 | 55.5% |
反応手順
To a solution of 4-bromo-3-chloro-N-trimethylsilanylmethylthiobenzamide (Example I13) (4.43 g) in butanone (80 ml) was added potassium carbonate (2.73 g) and methyl iodide (1.02 ml). The reaction mixture was stirred at ambient temperature for 20 hours. The reaction mixture was concentrated and the residue purified by chromatography on silica gel (eluent: ethyl acetate/heptanes 1:5) to give of 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzimidic acid methyl ester (2.56 g). 1H-NMR (400 MHz, CDCl3): 7.55-7.15 (m, 3H), 3.55 (s, 2H), 1.98 (s, 3H), 0.00 (s, 9H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946447B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-9a6bbc02d5284deeb5a1a0a9201baa6a |
| 出典メモ | uspto-grants-2015_02 |