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Toluene → 2-Bromo-N-(3-methoxyphenyl)-N-methyl-propanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Propanoyl bromide, 2-bromo- | HCID 79047 | — |
| 反応物 | N-Methyl-m-anisidine | HCID 84349 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-N-(3-methoxyphenyl)-N-methyl-propanamide | HCID 19692936 | — |
反応手順
A solution of N-methyl-m-anisidine (265 g), triethylamine (269 ml) and toluene (550 ml) was stirred at 0° C. as 2-bromopropionyl bromide (202.6 ml) was added dropwise. The mixture was mechanically stirred overnight at room temperature. Water was added to the reaction and the aqueous layer was collected and extracted with ethyl acetate. All organic phases were combined, washed with 2N HCl, and dried (Na2SO4). The solvent was evaporated to yield an oil which was purified using Kugelrohr distillation. The distillate was dissolved in isopropyl ether. The solid product, 2-Bromo-N-(3-methoxyphenyl)-N-methyl-propanamide, m.p. 55°-56° C., crystallized from this solution.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726323 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-8b32fa3382184901ae70790edf4034ba |
| 出典メモ | uspto-grants-1998_03 |