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Chloroacetyl chloride → 2-chloro-N-(6-(2-chlorophenyl)-5-(4-chlorophenyl)-3-cyanopyridin-2-yl)-N-isobutylacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | 6-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-(isobutylamino)pyridine-3-carbonitrile | HCID 68715054 | — |
| 反応物 | HCID 178418689 | HCID 178418689 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-chloro-N-(6-(2-chlorophenyl)-5-(4-chlorophenyl)-3-cyanopyridin-2-yl)-N-isobutylacetamide | HCID 68718317 | — |
反応手順
To the product of Step A EXAMPLE 27 (300 mg) in THF (5.0 mL) was added MeMgBr (0.92 mL, 1.4 M solution in toluene/THF 3:1) at 0° C. The reaction stirred for 5 minutes before adding chloroacetyl chloride (0.08 mL). The reaction stirred about 7 hours and was diluted with EtOAc, washed with 2 M aqueous HCl and brine. The dried solution (Na2SO4) was concentrated and purified via flash chromatography on silica gel gradient eluted with 0-15% EtOAc in hexane affording the title compound. HPLC/MS: 471.9 (M+1), 473.9 (M+3); Rt=4.32 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728141B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-4b001e05ab75496f9739f145f583a4bb |
| 出典メモ | uspto-grants-2010_06 |