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Methylamine → 3-(4-Bromo-phenyl)-3-(4-chloro-phenyl)-N-methyl-propionamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 1-(3-Dimethylaminopropyl)ethylcarbodiimide hydrochloride | HCID 21982921 | — |
| 反応物 | 3-(4-Bromo-phenyl)-3-(4-chloro-phenyl)-propionic acid | HCID 57691396 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(4-Bromo-phenyl)-3-(4-chloro-phenyl)-N-methyl-propionamide | HCID 59331970 | — |
反応手順
A mixture of 3-(4-bromo-phenyl)-3-(4-chloro-phenyl)-propionic acid (0.25 g, 0.74 mmol) and 1-hydroxybenatriazole (0.12 g, 0.88 mmol) in dichloromethane (3 ml) was stirred for 15 minutes before addition of methylamine (40% solution in water, 0.110, 1.47 mmol) and 1-(3-dimethylaminopropyl)-ethylcarbodiimide hydrochloride (0.17 g, 0.88 mmol). The reaction mixture was stirred for 16 hours, solvent removed under reduced pressure and the residue partitioned between ethyl acetate and 1N HCl. The organic layer was separated, washed with saturated sodium hydrogen carbonate, brine, dried (MgSO4), filtered and concentrated to yield the title compound which was used in the next step without further purification. LC/MS: (PS-A2) Rt 3.20 [M+H]+ 353.95.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541461B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-bcb8c9e4374648ec93c815f1d0e4a343 |
| 出典メモ | uspto-grants-2013_09 |