反応式
Clc1ccnc(Cl)c1.Cn1nccc1N>C1COCCO1.CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].[Pd]>Cn1nccc1Nc1cc(Cl)ccn1参加物
反応物 2
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 105 °C
実験手順
TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (251 mg, 0.27 mmol) was [AP-added] to 2,4-dichloropyridine (1000mg, 6.76 mmol), 1-methyl-1H-pyrazol-5-amine (722 mg, 7.43 mmol), cesium carbonate (3302 mg, 10.14 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (461 mg, 0.80 mmol) in 1,4-dioxane (75 mL) warmed to 105ºC over a period of 21 hours under nitrogen. The reaction mixture was evaporated to dryness and redissolved in DCM (50 mL), and sequentially with water (25 mL). The organic layer was filtered using phase separating paper and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 3% MeOH in DCM. Pure fractions were evaporated to dryness to afford 4-chloro-N-(1-methyl-1H-pyrazol-5-yl)pyridin-2-amine (710 mg, 50.4 %) as a brown oil.
出典と根拠
- ORDレコード
- ord-90d260fec9dd4d62a1593e5cdff9b43a
- 出典データセット
- 750 AstraZeneca ELN dataset
- 元リンク
- 出典を表示
関連ノート
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