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Chloroacetyl chloride → N-(2'-Chloro-6'-methylphenyl)-N-chloroacetyl-4-methylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | N-(2'-chloro-6'-methylphenyl)-4-methylaniline | HCID 57952145 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(2'-Chloro-6'-methylphenyl)-N-chloroacetyl-4-methylaniline | HCID 57952152 | 77.9% |
反応手順
The solution of N-(2′-chloro-6′-methylphenyl)-4-methylaniline (1.4 g) in 2.21 g chloroacetylchloride is heated to 90° C. for 4 h. The mixture is diluted with toluene (25 ml), cooled to room temperature and washed with aqu. sodium carbonate. The organic phase is dried, evaporated and the residue is subjected to flash chromatography [57 g silica, toluene and toluene/ethylacetate (98:2)] to afford 1.45 g of N-(2′-Chloro-6′-methylphenyl)-N-chloroacetyl-4-methylaniline which is crystallised from heptane, mp: 113-114° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07906677B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-a3456b5d6a45462da116fb640b9a79d2 |
| 出典メモ | uspto-grants-2011_03 |