関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Methyl-4-(tributylstannyl)pyridine | HCID 21660574 | — |
| 反応物 | Tert-butyl 2-(4-chloro-3-cyanophenyl)acetate | HCID 58447897 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Tert-butyl 2-(3-cyano-4-(2-methylpyridin-4-yl)phenyl)acetate | HCID 58447938 | — |
反応手順
A mixture of tert-butyl 2-(4-chloro-3-cyanophenyl)acetate 111-7 (572 mg, 2.28 mmol), 2-methyl-4-(tributylstannyl)pyridine 111-8 (870 mg, 2.28 mmol) and Pd(PPh3)4 (220 mg, 0.2 mmol) and DMF (9 mL) was stirred at 120° C. for 10 hours under argon. After cooling to room temperature, the mixture was diluted with ethyl acetate, washed with saturated aqueous Na2S2O3 solution, water and brine, dried over Na2SO4, and concentrated to dryness by rotary evaporation. The crude was purified by silica gel flash chromatography, eluted with 5% methanol in dichloromethane to give tert-butyl 2-(3-cyano-4-(2-methylpyridin-4-yl)phenyl)acetate 111-9 as a yellow oil. MS m/z 309.2 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09238646B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-2cab6c97868a4e3b91a2c368f2fa615c |
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| 出典メモ | uspto-grants-2016_01 |
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