2-Bromo-3-chloropyridine → HCID 178418209、化合物
反応式
CN1CC(N)C1.Cl.Clc1cccnc1Br>CC(C)(C)[O-].Cc1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.[Na+].[Pd].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>CN1CC(Nc2ncccc2Cl)C1参加物
反応条件
- 温度
- 115 °C
実験手順
Pd2(dba)3 (0.018 g, 0.02 mmol), 2,2'-bis(diphenylphosphanyl)-1,1'-binaphthalene (BINAP) (0.024 g, 0.04 mmol) and toluene (4 mL) was added to a flask. 2-bromo-3-chloropyridine (0.5 g, 2.60 mmol), 1-methylazetidin-3-amine hydrochloride (0.414 g, 3.38 mmol) and sodium 2-methylpropan-2-olate (0.624 g, 6.50 mmol) was added, the mixture bubbled with N2 for 5 min, then the reaction was heated to 115 °C in an oil-bath under nitrogen for 2h, then to rt over night. The reaction was cooled to rt and the solvent was evaporated. The residue was purified by automated flash chromatography on a 100g column. A gradient from 10% to 100% of EtOAc (with 2% TEA) in heptane over 25CV was used as mobile phase. The product was collected using the wavelength 243 and 308 nm. No product found in any fractions. Reaction discarded.
出典と根拠
- ORDレコード
- ord-9a8d9c41c7b94faa97814a83a1ab2d95
- 出典データセット
- 750 AstraZeneca ELN dataset
- 元リンク
- 出典を表示
反応ノート
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