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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N-(2-Bromobenzyl)-2,2-diethoxyacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Bromobenzylamine | HCID 334072 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | Sodium diethoxyacetate | HCID 23663712 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(2-Bromobenzyl)-2,2-diethoxyacetamide | HCID 59636401 | — |
反応手順
1-[3-(Dimethylamino)propyl]-3-ethylcarbodiimide (1.15 g, 6.00 mmol) was added to a mixture of 2-bromobenzylamine (0.744 g, 4.00 mmol), sodium 2,2-diethoxyacetate (0.816 g, 4.80 mmol), 1-hydroxybenzotriazole hydrate (0.919 g, 6.00 mmol) and Hunig's base (1.53 mL, 8.80 mmol) in DMF (10 mL) with stirring. After 18 hours at room temperature, the mixture was partitioned between water and ethyl acetate. The organic layer was washed successively with 2 M HCl, saturated sodium bicarbonate solution and brine, then dried (Na2SO4) and concentrated to a viscous colourless oil (1.02 g, 81%). LC-MS (1) Rt==2.23 min; m/z (ESI+) 316 & 318 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530468B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-68febdba4f2f472fbba15dc96a7fbf5f |
| 出典メモ | uspto-grants-2013_09 |