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Sodium Acetate → 2-Bromo-4-{[(trimethysilyl)methyl]carbamoyl}benzyl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 3-bromo-4-(bromomethyl)-N-[(trimethysilyl)methyl]benzamide | HCID 58092079 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 2-Bromo-4-{[(trimethysilyl)methyl]carbamoyl}benzyl acetate | HCID 58092081 | 39.1% |
反応手順
A mixed solution of sodium acetate (2.8 g), 3-bromo-4-(bromomethyl)-N-[(trimethysilyl)methyl]benzamide (6.5 g) in DMF (30 ml) was stirred for 3 hours at 70° C. The reaction liquor was returned to room temperature and diluted with t-butyl methyl ether. The mixture was washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After separating the drying agent by filtration, the reaction liquor was distilled off under reduced pressure, and the resulting mixture was purified by silica gel chromatography, to obtain 2-bromo-4-{[(trimethysilyl)methyl]carbamoyl}benzyl acetate (2.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08304371B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-71f4618851ce4e068720ce3034ccca9f |
| 出典メモ | uspto-grants-2012_11 |