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Chloroacetyl chloride → n-(5-Bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Amino-5-bromo-3-methylpyridine | HCID 137934 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | n-(5-Bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide | HCID 52228026 | — |
反応手順
1.75 mL (22 mmol) chloroacetyl chloride are added to a solution, cooled to 0° C., of 3.74 g (20 mmol) 2-amino-5-bromo-3-methylpyridine in 50 mL DCM and then 6.1 mL (44 mmol) triethylamine are slowly added dropwise. After the addition has ended the ice bath is removed and the reaction mixture is stirred for 4 h at RT. It is poured onto water, extracted exhaustively with DCM, the combined organic phases are washed with water and saturated NaCl solution and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography (silica gel, cyc/EtOAc 2:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08618132B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-4aede1005bfe4e03826578031574b8ca |
| 出典メモ | uspto-grants-2013_12 |